Structural diversity for phosphine complexes of stibenium and stibinidenium cations
Saurabh S. Chitnis; Brendan Peters; Eamonn Conrad; Neil Burford; Robert McDonald; Michael J. Ferguson; Chem.Commun. 47 (2011) 12331–; doi:10.1039/c1cc15693d

data_7107065
_publ_section_title
;
 Structural diversity for phosphine complexes of stibenium and
 stibinidenium cations
;
_journal_coden_Cambridge         0182
_journal_name_full               Chem.Commun.
_journal_page_first              12331
_journal_paper_doi               10.1039/c1cc15693d
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C26 H24 Cl2 P2 Sb, C H2 Cl2, Al Cl4'
_chemical_formula_sum            'C27 H26 Al Cl8 P2 Sb'
_chemical_formula_weight         844.75
_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                74.3015(3)
_cell_angle_beta                 71.3838(3)
_cell_angle_gamma                87.5567(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5270(3)
_cell_length_b                   12.8155(3)
_cell_length_c                   14.0046(3)
_cell_measurement_reflns_used    9547
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      2.50
_cell_volume                     1721.72(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-2008 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0142
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15558
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    1.559
_exptl_absorpt_correction_T_max  0.7930
_exptl_absorpt_correction_T_min  0.7060
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.346
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         7895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+1.3868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0582
_reflns_number_gt                7215
_reflns_number_total             7895
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1cc15693d.txt
_cod_data_source_block           dal1166
_cod_database_code               7107065