Dimeric Bridged and Chelated Alkali Metal (Li and Na) Bis(iminophosphorano)methanide Complexes with Contrasting Structures
Ruppa P. Kamalesh Babu; Kasani Aparna; Robert McDonald; Ronald G. Cavell; Inorganic Chemistry 39 (2000) 4981–4984; doi:10.1021/ic991364z

data_4321488
_publ_section_title
;
 Dimeric Bridged and Chelated Alkali Metal (Li and Na)
 Bis(iminophosphorano)methanide Complexes with Contrasting Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4981
_journal_page_last               4984
_journal_paper_doi               10.1021/ic991364z
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C69 H86 N4 Na2 P4 Si4'
_chemical_formula_weight         1253.64
_chemical_name_systematic
; 
 ? 
;
_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           SHELXL-97
_cell_angle_alpha                76.1521(15)
_cell_angle_beta                 86.5411(16)
_cell_angle_gamma                73.2969(13)
_cell_formula_units_Z            2
_cell_length_a                   12.3907(10)
_cell_length_b                   14.5179(11)
_cell_length_c                   21.3739(14)
_cell_measurement_reflns_used    3979
_cell_measurement_temperature    193(2)
_cell_volume                     3575.5(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_sigmaI/netI    0.1294
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19445
_diffrn_reflns_theta_full        25.73
_diffrn_reflns_theta_max         25.73
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  0.9683
_exptl_absorpt_correction_T_min  0.9303
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.151
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         13529
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.120
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0890P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1654
_refine_ls_wR_factor_ref         0.1861
_reflns_number_gt                7704
_reflns_number_total             13529
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991364z_1.cif
_cod_data_source_block           '[Na{?2-?N,?N-CH(Ph2P=NSiMe3)2}]2'
_cod_database_code               4321488