Alkali metal‒1-azaallyl complexes: X-ray crystallographic, NMR spectroscopic and ab initio calculational studies
Armstrong, David R.; Clegg, William; Dunbar, Lorraine; Liddle, Stephen T.; MacGregor, Murray; Mulvey, Robert E.; Reed, David; Quinn, Susan A.; Journal of the Chemical Society, Dalton Transactions  (1998) 3431–; doi:10.1039/a805523h

data_7028150
_publ_section_title
;
 Alkali metal--1-azaallyl complexes: X-ray crystallographic, NMR
 spectroscopic and ab initio calculational studies
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3431
_journal_paper_doi               10.1039/a805523h
_journal_year                    1998
_chemical_formula_sum            'C24 H60 Li2 N8 O2 P2'
_chemical_formula_weight         568.62
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 101.871(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.163(2)
_cell_length_b                   15.1740(14)
_cell_length_c                   10.1786(9)
_cell_measurement_reflns_used    5599
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.24
_cell_volume                     3501.0(5)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0693
_diffrn_reflns_av_sigmaI/netI    0.1074
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21473
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.86
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         8260
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1535
_refine_ls_R_factor_gt           0.0645
_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^)+(0.0682P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1586
_reflns_number_gt                4181
_reflns_number_total             8260
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            h805523sup1.cif
_cod_data_source_block           3
_cod_original_cell_volume        3501.0(6)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7028150