Oxonium (dihydrogen 1-aminoethane-1,1-diyldiphosphonato-κ^2^<i>N</i>,<i>O</i>)[hydrogen (1-amino-1-phosphonoethyl)phosphonato-κ^2^<i>N</i>,<i>O</i>]palladium(II) trihydrate
Dudko, Anatolij; Bon, Vladimir; Kozachkova, Alexandra; Tsaryk, Natalia; Pekhnyo, Vasily; Acta Crystallographica Section E 66 (2010) m170–m171; doi:10.1107/S1600536810000930

data_2225001
_publ_section_title
;
 Oxonium (dihydrogen
 1-aminoethane-1,1-diyldiphosphonato-\k^2^<i>N</i>,<i>O</i>)[hydrogen
 (1-amino-1-phosphonoethyl)phosphonato-\k^2^<i>N</i>,<i>O</i>]palladium(II)
 trihydrate
;
_journal_coeditor_code           HG2625
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m170
_journal_page_last               m171
_journal_paper_doi               10.1107/S1600536810000930
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'(H3 O) [Pd (C2 H7 N O6 P2) (C2 H8 N O6 P2)] , 3H2 O'
_chemical_formula_moiety         'H3 O + , C4 H15 N2 O12 P4 Pd - , 3H2 O'
_chemical_formula_sum            'C4 H24 N2 O16 P4 Pd'
_chemical_formula_weight         586.53
_chemical_melting_point          542
_chemical_name_systematic
;
Oxonium (dihydrogen
1-aminoethane-1,1-diyldiphosphonato-\k^2^<i>N</i>,<i>O</i>)[hydrogen
(1-amino-1-phosphonoethyl)phosphonato-\k^2^<i>N</i>,<i>O</i>]palladium(II)
trihydrate
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                   9.9412(2)
_cell_length_b                   9.0941(2)
_cell_length_c                   19.9004(3)
_cell_measurement_reflns_used    9199
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.67
_cell_measurement_theta_min      3.03
_cell_volume                     1799.12(6)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0129
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            53680
_diffrn_reflns_theta_full        30.74
_diffrn_reflns_theta_max         30.74
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    1.472
_exptl_absorpt_correction_T_max  0.8227
_exptl_absorpt_correction_T_min  0.5360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.607
_refine_ls_abs_structure_details
'racemic twin (Flack, 1983), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   0.362(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         5568
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0146
_refine_ls_R_factor_gt           0.0145
_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^)+(0.0254P)^2^+0.6821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0407
_refine_ls_wR_factor_ref         0.0407
_reflns_number_gt                5545
_reflns_number_total             5568
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2625.cif
_cod_data_source_block           I
_cod_database_code               2225001
_cod_database_fobs_code          2225001