Novel ion pairs obtained from the reaction of titanium(IV) halides with simple arsane ligands
Thomas, Tegan; Pugh, David; Parkin, Ivan P.; Carmalt, Claire J.; Acta Crystallographica Section C 67 (2011) m96–m99; doi:10.1107/S0108270111006639

data_2018035
_publ_section_title
;
 Novel ion pairs obtained from the reaction of titanium(IV) halides
 with simple arsane ligands
;
_journal_coeditor_code           GG3254
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m96
_journal_page_last               m99
_journal_paper_doi               10.1107/S0108270111006639
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C18 H15 As Br)2 [Ti2 Br8 O]'
_chemical_formula_moiety         '2(C18 H15 As Br +), Br8 O Ti2 2-'
_chemical_formula_sum            'C36 H30 As2 Br10 O Ti2'
_chemical_formula_weight         1523.34
_chemical_name_systematic
;
bis[bromidotriphenylarsenium(V)]
di-\m-bromido-\m-oxido-bis[tribromidotitanium(IV)]
;
_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           SHELXL97
_cell_angle_alpha                81.2100(10)
_cell_angle_beta                 83.017(2)
_cell_angle_gamma                67.4480(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4991(2)
_cell_length_b                   10.7921(3)
_cell_length_c                   21.5971(6)
_cell_measurement_reflns_used    40727
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2228.12(10)
_computing_cell_refinement
;
DENZO (Otwinowski & Minor, 1997) and COLLECT (Nonius, 1998)
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
DENZO (Otwinowski & Minor, 1997) and COLLECT (Nonius, 1998)
;
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
PLATON (Spek, 2009), WinGX (Farrugia, 1999) and enCIFer (Allen
<i>et al.</i>, 2004)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 4096x4096
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type
'Bruker Nonius APEXII CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker--Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            33234
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.94
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.828
_exptl_absorpt_correction_T_max  0.4779
_exptl_absorpt_correction_T_min  0.2207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.061
_refine_diff_density_min         -1.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         10149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0000P)^2^+15.7068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.1011
_reflns_number_gt                7721
_reflns_number_total             10149
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg3254.cif
_cod_data_source_block           III
_cod_database_code               2018035
_cod_database_fobs_code          2018035