Iminophosphine Cycloaddition Reactions of a Diazaphosphoniaaluminatacyclobutane and a Novel Intramolecular Phosphiridine P\ρightarrowP Coordination
Neil Burford; Daren J. LeBlanc; Inorganic Chemistry 38 (1999) 2248–2249; doi:10.1021/ic9813718

data_4322022
_publ_contact_author_address
;  Department of Chemistry
   Dalhousie University
   Halifax, NS B3H 4J3
   CANADA
;
_publ_contact_author_email       burford@chem1.chem.dal.ca
_publ_contact_author_fax         '(902) 494-1310'
_publ_contact_author_name        'Neil Burford'
_publ_contact_author_phone       '(902) 494-3681'
_publ_section_title
;
 Iminophosphine Cycloaddition Reactions of a
 Diazaphosphoniaaluminatacyclobutane and a Novel Intramolecular
 Phosphiridine P\\rightarrowP Coordination
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2248
_journal_page_last               2249
_journal_paper_doi               10.1021/ic9813718
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         'C24 H20 P1 1+, C12 H36 Al1 Cl2 N4 P2 Si4 1-'
_chemical_formula_sum            'C36 H56 Al Cl2 N4 P3 Si4'
_chemical_formula_weight         848.00
_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                 98.6260(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6485(3)
_cell_length_b                   18.6224(4)
_cell_length_c                   17.3207(4)
_cell_measurement_reflns_used    46910
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      4.10
_cell_volume                     4671.47(18)
_computing_cell_refinement       'DENZO-SMN (Nonius, 1997)'
_computing_data_collection       'KappaCCD Server software (Nonius, 1997)'
_computing_data_reduction        'DENZO-SMN (Nonius, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.2
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1\% rotations on \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube (50 kV, 23 mA)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0870
_diffrn_reflns_av_sigmaI/netI    0.0675
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46910
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         4.10
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  0.9292
_exptl_absorpt_correction_T_min  0.9221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Nonius, 1997'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.737
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         9514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1361
_reflns_number_gt                6404
_reflns_number_total             9514
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic9813718_2.cif
_cod_data_source_block           djl38b_[Ph~4~P][2]
_cod_database_code               4322022