Monomeric Alkali Metal (Li, Na, K) Complexes of Bis(iminophosphorano)methanides
Kamalesh Babu, Ruppa P.; Aparna, Kasani; McDonald, Robert; Cavell, Ronald G.; Organometallics 20 (2001) 1451–; doi:10.1021/om000982g

data_4077256
_publ_section_title
;
 Monomeric Alkali Metal (Li, Na, K) Complexes of
 Bis(iminophosphorano)methanides
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1451
_journal_paper_doi               10.1021/om000982g
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C39 H55 N2 Na O2 P2 Si2'
_chemical_formula_weight         724.96
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 96.104(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.412(14)
_cell_length_b                   10.276(6)
_cell_length_c                   19.489(14)
_cell_measurement_temperature    193(2)
_cell_volume                     4065(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1093
_diffrn_reflns_av_sigmaI/netI    0.1436
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12494
_diffrn_reflns_theta_full        25.74
_diffrn_reflns_theta_max         25.74
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_T_max  0.9875
_exptl_absorpt_correction_T_min  0.9511
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.1375
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1587
_reflns_number_gt                1932
_reflns_number_total             3878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000982g.cif
_cod_data_source_block           rgc9905_Compound_4
_cod_database_code               4077256