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_1558076
_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         'C34 H72 B4 Dy2 O2'
_chemical_formula_sum            'C34 H72 B4 Dy2 O2'
_chemical_formula_weight         881.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-10
_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                99.987(4)
_cell_angle_beta                 105.704(4)
_cell_angle_gamma                107.788(4)
_cell_formula_units_Z            2
_cell_length_a                   10.0067(5)
_cell_length_b                   14.2962(7)
_cell_length_c                   16.3689(8)
_cell_measurement_reflns_used    5651
_cell_measurement_temperature    220
_cell_measurement_theta_max      71.0180
_cell_measurement_theta_min      4.7850
_cell_volume                     2061.0(2)
_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      220
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_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    -95.00 -17.00   1.00    8.21    --  -36.75 -77.00 -90.00   78
  2  \w    -24.00  30.00   1.00    8.21    --  -36.75  77.00  30.00   54
  3  \w     68.00 101.00   1.00    8.21    --   36.75  77.00 120.00   33
  4  \w    -24.00  75.00   1.00    8.21    --   36.75 -99.00 120.00   99
  5  \w      9.00  40.00   1.00    8.21    --   36.75 -19.00 120.00   31
  6  \w    -21.00  76.00   1.00    8.21    --   36.75 -99.00   0.00   97
  7  \w     18.00  98.00   1.00    8.21    --   36.75  77.00-150.00   80
  8  \w     39.00 118.00   1.00   20.85    --  107.00 -45.00 -60.00   79
  9  \w     37.00 126.00   1.00   20.85    --  107.00 -30.00  90.00   89
 10  \w     39.00  82.00   1.00   20.85    --  107.00 -45.00  60.00   43
 11  \w     95.00 159.00   1.00   20.85    --  107.00  61.00 150.00   64
 12  \w     64.00 119.00   1.00   20.85    --  107.00 -91.00 158.06   55
 13  \w     39.00 120.00   1.00   20.85    --  107.00 -89.00-143.34   81
 14  \w     36.00  79.00   1.00   20.85    --  107.00 -15.00-120.00   43
 15  \w    118.00 175.00   1.00   20.85    --  107.00  77.00-150.00   57
 16  \w     71.00 115.00   1.00   20.85    --  107.00 -90.00  42.18   44
 17  \w     52.00  84.00   1.00   20.85    --  107.00-111.00-180.00   32
 18  \w    116.00 145.00   1.00   20.85    --  107.00 -15.00-120.00   29
 19  \w     39.00 115.00   1.00   20.85    --  107.00 -45.00-150.00   76
 20  \w     86.00 176.00   1.00   20.85    --  107.00  30.00 -90.00   90
 21  \w     65.00 108.00   1.00   20.85    --  107.00 -91.00  82.63   43
 22  \w     72.00 129.00   1.00   20.85    --  107.00 -91.00 -61.17   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0505645000
_diffrn_orient_matrix_UB_12      -0.0849561000
_diffrn_orient_matrix_UB_13      -0.0864175000
_diffrn_orient_matrix_UB_21      0.1415532000
_diffrn_orient_matrix_UB_22      0.0574827000
_diffrn_orient_matrix_UB_23      -0.0182247000
_diffrn_orient_matrix_UB_31      0.0841516000
_diffrn_orient_matrix_UB_32      -0.0580518000
_diffrn_orient_matrix_UB_33      0.0506653000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13654
_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         71.386
_diffrn_reflns_theta_min         3.381
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.338
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50230
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         7793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0324P)^2^+0.7966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6524
_reflns_number_total             7793
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02033h2.cif
_cod_data_source_block           exp_1973
_cod_depositor_comments
;Adding full bibliography for 1558076--1558078.cif.

 Adding full bibliography for 1558076--1558078.cif.
;
_cod_original_cell_volume        2061.03(19)
_cod_database_code               1558076
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.113
_shelx_estimated_absorpt_t_min   0.068
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Secondary CH2 refined with riding coordinates:
 C27(H27a,H27b), C28(H28a,H28b), C29(H29a,H29b), C30(H30a,H30b), C31(H31a,
 H31b), C32(H32a,H32b), C33(H33a,H33b), C34(H34a,H34b)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C10(H10)
2.c Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C16(H16a,H16b,
 H16c), C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), C20(H20a,H20b,H20c), C21(H21a,
 H21b,H21c), C22(H22a,H22b,H22c), C24(H24a,H24b,H24c), C25(H25a,H25b,H25c),
 C26(H26a,H26b,H26c)
;
_shelx_res_checksum              33817
_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 1.820
_oxdiff_exptl_absorpt_empirical_full_min 0.730