Syntheses and X-ray Structures of Novel Main Group Bis(dialkylamino)phosphinimides†
Schulz, S.; Raab, M.; Nieger, M.; Niecke, E.; Organometallics 19 (2000) 2616–; doi:10.1021/om000059e

data_4077478
_publ_section_title
;
 Syntheses and X-ray Structures of Novel Main Group
 Bis(dialkylamino)phosphinimides&#x2020;
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2616
_journal_paper_doi               10.1021/om000059e
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C27 H55 Al N3 P'
_chemical_formula_weight         479.69
_chemical_name_systematic
; 
 Bis(dicyclohexylamino)phosphoranimin-N-trimethylalane 
;
_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                95.024(3)
_cell_angle_beta                 105.047(4)
_cell_angle_gamma                111.370(4)
_cell_formula_units_Z            2
_cell_length_a                   10.5525(7)
_cell_length_b                   10.8527(9)
_cell_length_c                   15.0268(11)
_cell_measurement_reflns_used    7967
_cell_measurement_temperature    123(2)
_cell_volume                     1515.6(2)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       Collect
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 2 deg.'
_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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10221
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_T_max  '0.9864 (theor.)'
_exptl_absorpt_correction_T_min  '0.9470 (theor.)'
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.051
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5224
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0503P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                3635
_reflns_number_total             5224
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000059e.cif
_cod_data_source_block           compound_1
_cod_original_sg_symbol_H-M      'P-1 (No.2)'
_cod_database_code               4077478