Crystal structure of bis[(5-oxooxolan-3-yl)triphenylphosphanium] hexaiodidotellurate(IV)
Närhi, Sari M.; Oilunkaniemi, Raija; Laitinen, Risto S.; Acta Crystallographica Section E 70 (2014) o1241–; doi:10.1107/S1600536814023940

data_2240178
_publ_section_title
;
 Crystal structure of bis[(5-oxooxolan-3-yl)triphenylphosphanium]
 hexaiodidotellurate(IV)
;
_journal_coeditor_code           ZL2606
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1241
_journal_paper_doi               10.1107/S1600536814023940
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '2C22 H20 O2 P +, Te I6 2-'
_chemical_formula_moiety         '2(C22 H20 O2 P +), I6 Te 2-'
_chemical_formula_sum            'C44 H40 I6 O4 P2 Te'
_chemical_formula_weight         1583.70
_chemical_name_systematic
;
Bis[(5-oxooxolan-3-yl)triphenylphosphanium] hexaiodidotellurate(IV)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2013
_cell_angle_alpha                74.64(3)
_cell_angle_beta                 69.70(3)
_cell_angle_gamma                77.28(3)
_cell_formula_units_Z            1
_cell_length_a                   9.4479(19)
_cell_length_b                   11.022(2)
_cell_length_c                   13.259(3)
_cell_measurement_reflns_used    3957
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.744
_cell_measurement_theta_min      2.808
_cell_volume                     1236.1(5)
_computing_cell_refinement
;
DENZO-SMN (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Hooft, 1998)
;
_computing_data_reduction
;
DENZO-SMN (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11104
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.744
_diffrn_reflns_theta_min         2.808
_exptl_absorpt_coefficient_mu    4.451
_exptl_absorpt_correction_T_max  0.92715
_exptl_absorpt_correction_T_min  0.54299
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
(XPREP in SHELXTL; Sheldrick, 2008)
;
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    2.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.802
_refine_diff_density_min         -1.035
_refine_ls_extinction_coef       0.0026(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2013 (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4557
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+2.1829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0775
_reflns_number_gt                3957
_reflns_number_total             4557
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zl2606sup1.cf
_cod_data_source_block           I
_cod_database_code               2240178
_cod_database_fobs_code          2240178
_shelx_estimated_absorpt_t_min   0.402
_shelx_estimated_absorpt_t_max   0.470
_shelx_hkl_checksum              77628
_shelx_res_checksum              18351
_shelxl_version_number           .2013