Crystal structures and hydrogen bonding in the isotypic series of hydrated alkali metal (K, Rb and Cs) complexes with 4-aminophenylarsonic acid
Smith, Graham; Wermuth, Urs D.; Acta Crystallographica Section E 73 (2017) 203–208; doi:10.1107/S2056989017000445

data_2242029
_publ_section_title
;
 Crystal structures and hydrogen bonding in the isotypic series of
 hydrated alkali metal (K, Rb and Cs) complexes with 4-aminophenylarsonic
 acid
;
_journal_coeditor_code           WM5350
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              203
_journal_page_last               208
_journal_paper_doi               10.1107/S2056989017000445
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Cs (C6 H7 As N O3) (H2 O)1.5]'
_chemical_formula_moiety         'C6 H7 As N O3, Cs, 1.5(H2 O)'
_chemical_formula_sum            'C6 H10 As Cs N O4.5'
_chemical_formula_weight         375.98
_chemical_name_common            'caesium <i>p</i>-arsanilate sesquihydrate'
_chemical_name_systematic
;
Poly[di-\m~3~-4-aminophenylarsonato-tri-\m~2~-aqua-dicaesium]
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.650(3)
_cell_length_b                   10.4373(9)
_cell_length_c                   8.3992(7)
_cell_measurement_reflns_used    1999
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.94
_cell_measurement_theta_min      3.98
_cell_volume                     2160.9(4)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008) within WinGX (Farrugia, 2012)
;
_computing_structure_solution
;
SIR92 (Altomare <i>et al.</i>, 1993)
;
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 16.077
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-S CCD-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance Mo X-ray source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4941
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.25
_diffrn_reflns_theta_min         3.16
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.457
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.689
_refine_diff_density_min         -1.003
_refine_ls_abs_structure_details
;
Flack (1983), 1405 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.10(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1883
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1178P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1597
_reflns_number_gt                1787
_reflns_number_total             1883
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm5350sup1.cif
_cod_data_source_block           III
_cod_database_code               2242029
_cod_depositor_comments
;

2017-05-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C12 H20 As2 Cs2 N2 O9'
_cod_original_formula_weight         751.96
_cod_original_formula_moiety         'C12 H20 As2 Cs2 N2 O9'
_cod_original_formula_units_Z            4
_cod_database_fobs_code 2242029