The reactions of alkylamino substituted phosphines with I2 and (Ph2Se2I2)2: structural features of alkylamino phosphonium cations
Barnes, Nicholas A.; Godfrey, Stephen M.; Halton, Ruth T. A.; Mushtaq, Imrana; Pritchard, Robin G.; Dalton Transactions  (2008) 1346–1354; doi:10.1039/b713640d

data_7003187
_publ_section_title
;
 The reactions of alkylamino substituted phosphines with I2 and
 (Ph2Se2I2)2: structural features of alkylamino phosphonium cations
;
_journal_issue                   10
_journal_name_full               'Dalton Transactions'
_journal_page_first              1346
_journal_page_last               1354
_journal_paper_doi               10.1039/b713640d
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C12 H24 I2 N3 P1'
_chemical_formula_sum            'C12 H24 I2 N3 P'
_chemical_formula_weight         495.11
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2006-08-08T11:09:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.655(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7268(4)
_cell_length_b                   21.6107(9)
_cell_length_c                   9.3212(4)
_cell_measurement_reflns_used    2947
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.5
_cell_measurement_theta_min      2
_cell_measurement_wavelength     0.71073
_cell_volume                     1757.17(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.848478E-1
_diffrn_orient_matrix_UB_12      0.522E-4
_diffrn_orient_matrix_UB_13      -0.698484E-1
_diffrn_orient_matrix_UB_21      0.768127E-1
_diffrn_orient_matrix_UB_22      -0.39649E-2
_diffrn_orient_matrix_UB_23      0.811816E-1
_diffrn_orient_matrix_UB_31      -0.65098E-2
_diffrn_orient_matrix_UB_32      -0.461032E-1
_diffrn_orient_matrix_UB_33      -0.70607E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14127
_diffrn_reflns_reduction_process
;
Scaled and merged with SORTAV
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        26.5
_diffrn_reflns_theta_max         26.5
_diffrn_reflns_theta_min         3.24
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.661
_exptl_absorpt_correction_T_max  0.8381
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.16
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+11.3854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                2606
_reflns_number_total             3496
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b713640d.txt
_cod_data_source_block           s3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7003187