Synthesis and reactivity of cyclo-tetra(stibinophosphonium) tetracations: redox and coordination chemistry of phosphine‒antimony complexes
Chitnis, Saurabh S.; Robertson, Alasdair P. M.; Burford, Neil; Weigand, Jan J.; Fischer, Roland; Chem. Sci. 6 (2015) 2559–; doi:10.1039/C4SC03939D

data_1518666
_publ_section_title
;
 Synthesis and reactivity of cyclo-tetra(stibinophosphonium) tetracations:
 redox and coordination chemistry of phosphine--antimony complexes
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              2559
_journal_paper_doi               10.1039/C4SC03939D
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C6 H16 F P2 Sb, 2(C F3 O3 S)'
_chemical_formula_sum            'C8 H16 F7 O6 P2 S2 Sb'
_chemical_formula_weight         589.02
_chemical_name_systematic        '[(dmpe)SbF][OTf]2'
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Hygroscopic'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2014-12-18 deposited with the CCDC.
2015-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.2600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5029(6)
_cell_length_b                   8.9034(4)
_cell_length_c                   14.9927(6)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.12
_cell_measurement_theta_min      2.667
_cell_volume                     1920.41(14)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            52517
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.304
_diffrn_reflns_theta_min         1.841
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.908
_exptl_absorpt_correction_T_max  0.8311
_exptl_absorpt_correction_T_min  0.6937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.037
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.131
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+1.2406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0490
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3773
_reflns_number_total             4279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc03939d2.cif
_cod_data_source_block           mo_vic1430_0m
_cod_depositor_comments
'Adding full bibliography for 1518666--1518671.cif.'
_cod_database_code               1518666
_shelx_estimated_absorpt_t_max   0.788
_shelx_estimated_absorpt_t_min   0.690
_olex2_refinement_description
;
;
_shelx_res_checksum              19755
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'