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_2018034
_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          '(C4 H12 As) [Ti2 Cl9]'
_chemical_formula_moiety         'C4 H12 As +, Cl9 Ti2 -'
_chemical_formula_sum            'C4 H12 As Cl9 Ti2'
_chemical_formula_weight         549.91
_chemical_name_systematic
;
<i>tert</i>-butylarsenium(V) tri-\m-chlorido-bis[trichloridotitanium(IV)]
;
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7061(15)
_cell_length_b                   17.855(3)
_cell_length_c                   10.4555(16)
_cell_measurement_reflns_used    2113
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      3.00
_cell_volume                     1812.0(5)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'SMART (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0642
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14917
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.995
_exptl_absorpt_correction_T_max  0.9611
_exptl_absorpt_correction_T_min  0.4350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2006)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.521
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         2329
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0353P)^2^+0.1344P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                1767
_reflns_number_total             2329
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg3254.cif
_cod_data_source_block           II
_cod_database_code               2018034
_cod_database_fobs_code          2018034