Bis(tetraphenylarsonium) hexafluoridotechnetate(IV) dihydrate: preparation, structure and spectroscopic analysis
Balasekaran, Samundeeswari Mariappan; Poineau, Frederic; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619014724

data_2021823
_publ_section_title
;
 Bis(tetraphenylarsonium) hexafluoridotechnetate(IV) dihydrate:
 preparation, structure and spectroscopic analysis
;
_journal_coeditor_code           DG3001
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619014724
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '(C24 H20 As)2 [Tc F6], 2H2 O1'
_chemical_formula_moiety         '2(C24 H20 As +), F6 Tc 2-, 2(H2 O)'
_chemical_formula_sum            'C48 H40 As2 F6 O2 Tc'
_chemical_formula_weight         1010.64
_chemical_name_common
;
Bis(tetraphenylarsonium) hexafluoridotechnetate(IV) dihydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                75.991(3)
_cell_angle_beta                 77.963(3)
_cell_angle_gamma                71.388(3)
_cell_formula_units_Z            2
_cell_length_a                   10.043(2)
_cell_length_b                   11.036(2)
_cell_length_c                   21.159(4)
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      28.4432
_cell_measurement_theta_min      2.2494
_cell_volume                     2134.3(7)
_computing_cell_refinement
;
SAINT (Bruker, 2017)
;
_computing_data_collection
;
APEX2 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_computing_molecular_graphics
;
<i>shelXle</i> (H\"ubschle <i>et al.</i>,  2011) and
DIAMOND (Brandenburg & Putz, 2005)
;
_computing_publication_material
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       ' '\f and \w scans'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30509
_diffrn_reflns_theta_full        28.44
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_min         1.98
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.941
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015; Bruker, 2017)
;
_exptl_crystal_colour            'translucent colourless'
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular box'
_exptl_crystal_F_000             1014
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.106
_refine_diff_density_max         0.850
_refine_diff_density_min         -1.279
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         10713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0241
_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^)+(0.0277P)^2^+1.0558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0608
_reflns_number_gt                9659
_reflns_number_total             10713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dg3001sup1.cif
_cod_data_source_block           I
_cod_database_code               2021823
_shelx_hkl_checksum              77039
_shelx_res_checksum              4066
_cod_database_fobs_code 2021823