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_7107063
_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_sum            'C31 H36 Al4 Cl11 P2 Sb'
_chemical_formula_weight         1090.16
_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                 98.272(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.299(2)
_cell_length_b                   10.3844(15)
_cell_length_c                   25.251(4)
_cell_measurement_reflns_used    9140
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.33
_cell_volume                     4229.4(10)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            32771
_diffrn_reflns_theta_full        26.55
_diffrn_reflns_theta_max         26.55
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    1.532
_exptl_absorpt_correction_T_max  0.7638
_exptl_absorpt_correction_T_min  0.4647
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.19
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as disordered
or partial-occupancy solvent pentane or dichloromethane chlorine or
carbon atoms were unsuccessful. The data were corrected for
disordered electron density through use of the SQUEEZE procedure
(Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194201)
as implemented in PLATON (Spek, A. L. Acta Crystallogr. 1990, A46,
C34; Spek, A. L. J. Appl. Cryst. 2003, 36, 713. PLATON - a
multipurpose crystallographic tool. Utrecht University, Utrecht, The
Netherlands). A total solvent-accessible void volume of 932 \%A3 with
a total electron count of 352 (consistent with 4 molecules each of
solvent dichloromethane and pentane, or 1 molecule of dichloromethane
and 1 molecule of pentane per formula unit of the [(dppm)SbCl][AlCl4]2
compound) was found in the unit cell.
;
_refine_diff_density_max         1.867
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         8740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0648P)^2^+6.7150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1257
_reflns_number_gt                7200
_reflns_number_total             8740
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1cc15693d.txt
_cod_data_source_block           dal1188
_cod_original_cell_volume        4229.3(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7107063