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_4321489
_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 Li2 N4 P4 Si4'
_chemical_formula_weight         1221.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.086(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5173(12)
_cell_length_b                   21.335(2)
_cell_length_c                   24.581(2)
_cell_measurement_reflns_used    6818
_cell_measurement_temperature    193(2)
_cell_volume                     7087.7(11)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0858
_diffrn_reflns_av_sigmaI/netI    0.1105
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            32936
_diffrn_reflns_theta_full        25.78
_diffrn_reflns_theta_max         25.78
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.215
_exptl_absorpt_correction_T_max  0.9621
_exptl_absorpt_correction_T_min  0.6401
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         13485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1407
_refine_ls_R_factor_gt           0.0807
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0932P)^2^+6.7197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2042
_refine_ls_wR_factor_ref         0.2281
_reflns_number_gt                7569
_reflns_number_total             13485
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991364z_2.cif
_cod_data_source_block           '[Li{?2-?N,?C,?N-CH(Ph2P=NSiMe3)2}]2'
_cod_database_code               4321489