Redetermination of tetraphenylarsonium <i>trans</i>-aquatetrachlorooxorhenate(V) at 100 K
Siczek, Miłosz; Lis, Tadeusz; Acta Crystallographica Section E 62 (2006) m358–m359; doi:10.1107/S1600536806001747

data_2208182
_publ_section_title
;
 Redetermination of tetraphenylarsonium
 <i>trans</i>-aquatetrachlorooxorhenate(V) at 100 K
;
_journal_coeditor_code           TK6296
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m358
_journal_page_last               m359
_journal_paper_doi               10.1107/S1600536806001747
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C24 H20 As) [Re Cl4 O (H2 O)]'
_chemical_formula_moiety         'C24 H20 As +, Cl4 H2 O2 Re -'
_chemical_formula_sum            'C24 H22 As Cl4 O2 Re'
_chemical_formula_weight         745.34
_chemical_name_common
'Tetraphenyloarsonium aqua-tetrachlorooxorhenate(V)'
_chemical_name_systematic
'Tetraphenyloarsonium aqua-tetrachlorooxorhenate(V)'
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.021(2)
_cell_length_b                   13.021(2)
_cell_length_c                   7.236(2)
_cell_measurement_reflns_used    20865
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.33
_cell_measurement_theta_min      3.2
_cell_volume                     1226.8(4)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction 2003)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'XP in SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Kuma KM-4-CCD \k-geometry'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_av_sigmaI/netI    0.020
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            19131
_diffrn_reflns_theta_full        35.0
_diffrn_reflns_theta_max         35.0
_diffrn_reflns_theta_min         3.2
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.747
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_correction_T_min  0.562
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.018
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'quadratic plates'
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.52
_refine_diff_density_min         -0.98
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         2671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.021
_refine_ls_R_factor_gt           0.018
_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^)+(0.0156P)^2^+0.8991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.038
_refine_ls_wR_factor_ref         0.039
_reflns_number_gt                2535
_reflns_number_total             2671
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk6296.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               2208182
_cod_database_fobs_code          2208182