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_4085292
_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            'C26 H49 K N2 O6 Si'
_chemical_formula_weight         552.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.2515(14)
_cell_length_b                   15.9542(15)
_cell_length_c                   26.784(3)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      2.45
_cell_volume                     6089.9(11)
_computing_cell_refinement       'Bruker SAINT, Ver 7.68a, 2009'
_computing_data_collection       'Bruker APEX2, Ver 2012.4-0, 2012'
_computing_data_reduction        'Bruker SAINT, Ver 7.68a, 2009'
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_computing_structure_solution    'Bruker SHELXS-97, Ver 2008/4'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Bruker 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  0.0590
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
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_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            58841
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.337
_diffrn_reflns_theta_min         2.061
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.8296
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       needle
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         7008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0358P)^2^+2.8910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                5346
_reflns_number_total             7008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501063h_si_002.cif
_cod_data_source_block           mrm48
_cod_depositor_comments
'Adding full bibliography for 4085286--4085294.cif.'
_cod_original_cell_volume        6090.0(10)
_cod_database_code               4085292
_shelx_estimated_absorpt_t_min   0.910
_shelx_estimated_absorpt_t_max   0.977
_shelxl_version_number           2013-3
_shelx_res_checksum              96381
_shelx_hkl_checksum              5055