An N,P-disubstituted-2-aminophosphaalkene and lithium and potassium complexes of the deprotonated ?phosphaamidinate? anion
Boer�, Ren� T.; Cole, Marcus L.; Junk, Peter C.; Masuda, Jason D.; Wolmersh�user, Gotthelf; Chemical Communications  (2004) 2564–2565; doi:10.1039/b408994d

data_7111414
_publ_section_title
;
 An N,P-disubstituted-2-aminophosphaalkene and lithium and potassium
 complexes of the deprotonated ?phosphaamidinate? anion
;
_journal_issue                   22
_journal_name_full               'Chemical Communications'
_journal_page_first              2564
_journal_page_last               2565
_journal_paper_doi               10.1039/b408994d
_journal_year                    2004
_chemical_formula_moiety         'C40 H57 K N O2 P'
_chemical_formula_sum            'C40 H57 K N O2 P'
_chemical_formula_weight         653.94
_chemical_melting_point          340
_chemical_name_common            ((K(N,P-Dipamidine)(THF))n).nTHF
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 131.306(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.6979(5)
_cell_length_b                   12.2579(4)
_cell_length_c                   24.1180(5)
_cell_measurement_temperature    223(2)
_cell_volume                     7927.8(4)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        X-Seed
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'psi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2154
_diffrn_reflns_av_sigmaI/netI    0.2164
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            43531
_diffrn_reflns_theta_full        27.85
_diffrn_reflns_theta_max         27.85
_diffrn_reflns_theta_min         2.82
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_T_max  0.9898
_exptl_absorpt_correction_T_min  0.9600
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'performed as part of the DENZO-SMN package'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'fine needle'
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         9321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.2776
_refine_ls_R_factor_gt           0.0892
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0833P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.2221
_reflns_number_gt                3166
_reflns_number_total             9321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b408994dsup1.cif
_cod_data_source_block           Cmpd_Cmpd#4
_cod_original_cell_volume        7927.8(3)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7111414