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_1558077
_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 H78 B2 Dy2'
_chemical_formula_sum            'C46 H78 B2 Dy2'
_chemical_formula_weight         977.70
_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             2020-01-10
_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                90
_cell_angle_beta                 107.3660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.31990(10)
_cell_length_b                   18.14390(10)
_cell_length_c                   19.6411(2)
_cell_measurement_reflns_used    15001
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      71.1040
_cell_measurement_theta_min      4.2400
_cell_volume                     4530.39(7)
_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_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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   -105.00 -78.00   1.00    8.97    --  -36.75-178.00  60.00   27
  2  \w    -84.00 -53.00   1.00    8.97    --  -36.75 178.00-150.00   31
  3  \w    -11.00  29.00   1.00    8.97    --  -36.75  57.00 -90.00   40
  4  \w   -106.00 -22.00   1.00    8.97    --  -36.75 -19.00  90.00   84
  5  \w    -21.00  76.00   1.00    8.97    --   36.75 -99.00-120.00   97
  6  \w     10.00 103.00   1.00    8.97    --   36.75  77.00   0.00   93
  7  \w    -22.00  74.00   1.00    8.97    --   36.75 -99.00  90.00   96
  8  \w     41.00 124.00   1.00   40.88    --  107.00 -45.00  90.00   83
  9  \w     46.00 121.00   1.00   40.88    --  107.00 -45.00-150.00   75
 10  \w     64.00 176.00   1.00   40.88    --  107.00   0.00-180.00  112
 11  \w     99.00 125.00   1.00   40.88    --  107.00  45.00-180.00   26
 12  \w    141.00 172.00   1.00   40.88    --  107.00  45.00-180.00   31
 13  \w     80.00 174.00   1.00   40.88    --  107.00  77.00-120.00   94
 14  \w     39.00 136.00   1.00   40.88    --  107.00 -91.00 -22.82   97
 15  \w    115.00 141.00   1.00   40.88    --  107.00  61.00 -90.00   26
 16  \w     84.00 110.00   1.00   40.88    --  107.00 -91.00 161.42   26
 17  \w     57.00 105.00   1.00   40.88    --  107.00 -91.00  68.60   48
 18  \w     73.00 100.00   1.00   40.88    --  107.00 -91.00-131.84   27
 19  \w     40.00 121.00   1.00   40.88    --  107.00 -45.00 -60.00   81
 20  \w     88.00 175.00   1.00   40.88    --  107.00  77.00-150.00   87
 21  \w     60.00 113.00   1.00   40.88    --  107.00 -91.00-109.01   53
 22  \w     49.00 142.00   1.00   40.88    --  107.00 -91.00 120.59   93
;
_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      -0.1007623000
_diffrn_orient_matrix_UB_12      0.0265627000
_diffrn_orient_matrix_UB_13      -0.0564832000
_diffrn_orient_matrix_UB_21      0.0043363000
_diffrn_orient_matrix_UB_22      -0.0674632000
_diffrn_orient_matrix_UB_23      -0.0466839000
_diffrn_orient_matrix_UB_31      -0.0672384000
_diffrn_orient_matrix_UB_32      -0.0441371000
_diffrn_orient_matrix_UB_33      0.0372649000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31291
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.204
_diffrn_reflns_theta_min         3.390
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.629
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46892
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         8690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.3733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0655
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7906
_reflns_number_total             8690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02033h2.cif
_cod_data_source_block           exp_1946
_cod_depositor_comments
;Adding full bibliography for 1558076--1558078.cif.

 Adding full bibliography for 1558076--1558078.cif.
;
_cod_database_code               1558077
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.272
_shelx_estimated_absorpt_t_min   0.177
_reflns_odcompleteness_completeness 99.95
_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.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C7(H7), C9(H9)
2.b Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c), C25(H25a,H25b,H25c), C35(H35a,H35b,H35c), C14(H14a,H14b,
 H14c), C24(H24a,H24b,H24c), C13(H13a,H13b,H13c), C12(H12a,H12b,H12c), C36(H36a,
 H36b,H36c), C18(H18a,H18b,H18c), C32(H32a,H32b,H32c), C21(H21a,H21b,H21c),
 C17(H17a,H17b,H17c), C22(H22a,H22b,H22c), C45(H45a,H45b,H45c), C33(H33a,H33b,
 H33c), C42(H42a,H42b,H42c), C20(H20a,H20b,H20c), C43(H43a,H43b,H43c), C34(H34a,
 H34b,H34c), C46(H46a,H46b,H46c), C16(H16a,H16b,H16c), C44(H44a,H44b,H44c)
;
_shelx_res_checksum              46846
_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 1.761
_oxdiff_exptl_absorpt_empirical_full_min 0.705