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_4085294
_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 H69 B K N2 O7.5'
_chemical_formula_weight         843.96
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                87.8620(8)
_cell_angle_beta                 76.9109(8)
_cell_angle_gamma                84.6246(8)
_cell_formula_units_Z            4
_cell_length_a                   13.7425(9)
_cell_length_b                   14.5093(9)
_cell_length_c                   24.4622(15)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      27.76
_cell_measurement_theta_min      2.20
_cell_volume                     4729.3(5)
_computing_cell_refinement       'Bruker SAINT 8.32b, 2012'
_computing_data_collection       'Bruker APEX2 2013.6-2, 2013'
_computing_data_reduction        'Bruker SAINT 8.32b, 2012'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL 2013/1'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0329
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49191
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         1.410
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.8141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2012/1'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       parallelpiped
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.492
_exptl_crystal_size_mid          0.291
_exptl_crystal_size_min          0.226
_refine_diff_density_max         1.178
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1074
_refine_ls_number_reflns         17929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0711
_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^)+(0.1114P)^2^+5.8931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1886
_refine_ls_wR_factor_ref         0.2074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13571
_reflns_number_total             17929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501063h_si_002.cif
_cod_data_source_block           cmk9
_cod_depositor_comments
'Adding full bibliography for 4085286--4085294.cif.'
_cod_original_formula_sum        'C48 H69 B K N2 O7.50'
_cod_database_code               4085294
_shelx_estimated_absorpt_t_min   0.924
_shelx_estimated_absorpt_t_max   0.964
_shelxl_version_number           2013-3
_shelx_res_checksum              17404
_shelx_hkl_checksum              29876