Synthesis and Magnetism of Neutral, Linear Metallocene Complexes of Terbium(II) and Dysprosium(II).
Gould, Colin A.; McClain, K. Randall; Yu, Jason M.; Groshens, Thomas J.; Furche, Filipp; Harvey, Benjamin G.; Long, Jeffrey R.; Journal of the American Chemical Society 141 (2019) 12967–12973; doi:10.1021/jacs.9b05816

data_4127839
_publ_section_title
;
 Synthesis and Magnetism of Neutral, Linear Metallocene Complexes of
 Terbium(II) and Dysprosium(II).
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12967
_journal_page_last               12973
_journal_paper_doi               10.1021/jacs.9b05816
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C40 H70 Dy'
_chemical_formula_sum            'C40 H70 Dy'
_chemical_formula_weight         713.46
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.917(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0200(5)
_cell_length_b                   13.0196(6)
_cell_length_c                   12.8467(8)
_cell_measurement_reflns_used    14809
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7510
_cell_measurement_theta_min      3.1360
_cell_volume                     1842.16(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_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      293(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -73.00  15.00   0.50    1.00    --    2.17 -47.00  -3.00  176
  2  \w    -25.00  45.00   0.50    1.00    --   -1.86  77.00-180.00  140
  3  \w    -45.00  21.00   0.50    1.00    --   -1.86 -77.00 -30.00  132
  4  \w    -45.00  21.00   0.50    1.00    --   -1.86 -77.00-180.00  132
  5  \w    -12.00  36.00   0.50    1.00    --    2.17 -99.00 150.00   96
  6  \w     10.00  36.00   0.50    1.00    --    2.17 -99.00  60.00   52
  7  \w     -7.00  34.00   0.50    1.00    --    2.17 -99.00   0.00   82
  8  \w    -11.00  36.00   0.50    1.00    --    2.17 -99.00 -30.00   94
  9  \w    -17.00  15.00   0.50    1.00    --    2.17  77.00 -60.00   64
 10  \w     -9.00  32.00   0.50    1.00    --    2.17 -99.00-180.00   82
 11  \w    -11.00  77.00   0.50    1.00    --    2.17  47.00 144.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            36352
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         2.862
_exptl_absorpt_coefficient_mu    2.052
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.188
_refine_diff_density_min         -1.585
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+7.1982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2894
_reflns_number_total             3365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05816_si_003.cif
_cod_data_source_block           rm7_91_3
_cod_database_code               4127839
_shelx_shelxl_version_number     2016/6
_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 Ternary CH refined with riding coordinates:
 C18(H18), C12(H12), C6(H6), C15(H15), C9(H9)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C16(H16A,H16B,
 H16C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C17(H17A,
 H17B,H17C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              4796
_shelx_hkl_checksum              94790
_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
;