Reactivity of the Ln2+Complexes [K(2.2.2-cryptand)][(C5H4SiMe3)3Ln]: Reduction of Naphthalene and Biphenyl
Kotyk, Christopher M.; MacDonald, Matthew R.; Ziller, Joseph W.; Evans, William J.; Organometallics 34 (2015) 2287–; doi:10.1021/om501063h

data_4085289
_publ_section_title
;
 Reactivity of the Ln2+Complexes [K(2.2.2-cryptand)][(C5H4SiMe3)3Ln]:
 Reduction of Naphthalene and Biphenyl
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2287
_journal_paper_doi               10.1021/om501063h
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C44 H70 Dy K N2 O6 Si2'
_chemical_formula_weight         980.80
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                105.0546(8)
_cell_angle_beta                 105.8184(9)
_cell_angle_gamma                94.8493(9)
_cell_formula_units_Z            2
_cell_length_a                   13.4991(10)
_cell_length_b                   13.8100(10)
_cell_length_c                   14.0940(10)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.29
_cell_volume                     2406.8(3)
_computing_cell_refinement       'Bruker SAINT 7.68a, 2009'
_computing_data_collection       'Bruker APEX2 2013.6-2, 2013'
_computing_data_reduction        'Bruker SAINT 7.68a, 2009'
_computing_molecular_graphics    'Bruker SHELXTL'
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_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23046
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.853
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.733
_exptl_absorpt_correction_T_max  0.9422
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_exptl_absorpt_correction_type   numerical
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_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1018
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         9720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0471P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8080
_reflns_number_total             9720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501063h_si_002.cif
_cod_data_source_block           cmk10
_cod_depositor_comments
'Adding full bibliography for 4085286--4085294.cif.'
_cod_database_code               4085289
_shelx_estimated_absorpt_t_min   0.659
_shelx_estimated_absorpt_t_max   0.804
_shelxl_version_number           2013-3
_shelx_res_checksum              47426
_shelx_hkl_checksum              52306