NMR, PGSE Diffusion, and X-ray Diffraction Studies of Lithium and Potassium Salts Derived from Diphenylphosphino(o-cyanophenyl)aniline and Their Crown Ether Complexes
Ignacio Fernández; Frank Breher; Paul S. Pregosin; Zhaofu Fei; Paul J. Dyson; Inorganic Chemistry 44 (2005) 7616–7623; doi:10.1021/ic050753s

data_4309749
_publ_contact_author_address
;
Department of Chemistry and Applied Biosciences
ETH Hoenggerberg
Wolgang-Pauli Str.
CH-8093 Zuerich
Switzerland
;
_publ_contact_author_email       pregosin@inorg.chem.ethz.ch
_publ_contact_author_fax         '(+41) 1 6331071'
_publ_contact_author_name        'Prof. Paul S. Pregosin'
_publ_section_title
;
NMR, PGSE Diffusion, and X-ray Diffraction Studies of Lithium and Potassium
Salts Derived from Diphenylphosphino(o-cyanophenyl)aniline and Their Crown
Ether Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7616
_journal_page_last               7623
_journal_paper_doi               10.1021/ic050753s
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C54 H60 K2 N4 O4 P2'
_chemical_formula_sum            'C54 H60 K2 N4 O4 P2'
_chemical_formula_weight         969.20
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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           'form.cif (version 2.0)'
_cell_angle_alpha                93.098(2)
_cell_angle_beta                 96.393(2)
_cell_angle_gamma                100.469(2)
_cell_formula_units_Z            1
_cell_length_a                   9.8819(7)
_cell_length_b                   10.7594(8)
_cell_length_c                   12.7185(9)
_cell_measurement_temperature    200(2)
_cell_volume                     1317.67(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep32 for Windows'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker AXS Apex with CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13810
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.287
_exptl_absorpt_correction_T_max  0.9555
_exptl_absorpt_correction_T_min  0.8442
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         6495
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0783
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1108P)^2^+0.8360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2019
_refine_ls_wR_factor_ref         0.2155
_reflns_number_gt                5261
_reflns_number_total             6495
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050753ssi20050512_050228.cif
_cod_data_source_block           Pamid
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4309749