Crystal structure and hydrogen bonding in the water-stabilized proton-transfer salt brucinium 4-aminophenylarsonate tetrahydrate
Smith, Graham; Wermuth, Urs D.; Acta Crystallographica Section E 72 (2016) 751–755; doi:10.1107/S2056989016006691

data_2241670
_publ_section_title
;
 Crystal structure and hydrogen bonding in the water-stabilized
 proton-transfer salt brucinium 4-aminophenylarsonate tetrahydrate
;
_journal_coeditor_code           LH5811
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              751
_journal_page_last               755
_journal_paper_doi               10.1107/S2056989016006691
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
'(C23 H27 N2 O4) [As (C6 H7 N) O2 (O H)], 4H2 O'
_chemical_formula_moiety         'C23 H27 N2 O4 +, C6 H7 As N O3 -, 4(H2 O)'
_chemical_formula_sum            'C29 H42 As N3 O11'
_chemical_formula_weight         683.58
_chemical_name_common            'brucinium <i>p</i>-arsanilate tetrahydrate'
_chemical_name_systematic
;
2,3-Dimethoxy-10-oxostrychnidinium 4-aminophenylarsonate tetrahydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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            4
_cell_length_a                   7.6553(3)
_cell_length_b                   12.3238(5)
_cell_length_c                   31.960(2)
_cell_measurement_reflns_used    2822
_cell_measurement_temperature    200.0(10)
_cell_measurement_theta_max      27.89
_cell_measurement_theta_min      3.38
_cell_volume                     3015.2(3)
_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      200.0(10)
_diffrn_detector_area_resol_mean 16.077
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device_type
'Oxford Diffraction Gemini-S CCD-detector diffractometer'
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            11983
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.52
_diffrn_reflns_theta_min         3.13
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.193
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.458
_refine_ls_abs_structure_details
;
Flack (1983), 3672 Friedel pairs
;
_refine_ls_abs_structure_Flack   -0.005(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6980
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0414P)^2^+0.2011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                5901
_reflns_number_total             6980
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5811sup1.cif
_cod_data_source_block           I
_cod_database_code               2241670
_cod_database_fobs_code          2241670