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_4085288
_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            'C48 H80 Ce K N2 O7 Si2'
_chemical_formula_weight         1032.54
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 96.954(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.549(2)
_cell_length_b                   15.974(3)
_cell_length_c                   25.192(4)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.44
_cell_volume                     5412.2(16)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2013.10-0, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
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_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.944
_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  0.0464
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            65452
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.066
_diffrn_reflns_theta_min         1.513
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_T_max  0.9115
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_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
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_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         13663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0488
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_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+2.9728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10803
_reflns_number_total             13663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501063h_si_002.cif
_cod_data_source_block           cmk17
_cod_depositor_comments
'Adding full bibliography for 4085286--4085294.cif.'
_cod_original_cell_volume        5412.3(16)
_cod_database_code               4085288
_shelx_estimated_absorpt_t_min   0.815
_shelx_estimated_absorpt_t_max   0.850
_shelxl_version_number           2014-2
_shelx_res_checksum              86542
_shelx_hkl_checksum              32060