Bis[(dimethylphosphoryl)methanaminium] tetrachloridopalladate(II)
Reiss, Guido J.; Acta Crystallographica Section E 69 (2013) m614–m615; doi:10.1107/S1600536813028067

data_2238815
_publ_section_title
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 Bis[(dimethylphosphoryl)methanaminium] tetrachloridopalladate(II)
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m614
_journal_page_last               m615
_journal_paper_doi               10.1107/S1600536813028067
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '(C3 H11 N O P)2 [Pd Cl4]'
_chemical_formula_moiety         '2(C3 H11 N O P +), Cl4 Pd 2-'
_chemical_formula_sum            'C6 H22 Cl4 N2 O2 P2 Pd'
_chemical_formula_weight         464.39
_chemical_name_systematic
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Bis[(dimethylphosphoryl)methanaminium] tetrachloridopalladate(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 110.110(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3600(3)
_cell_length_b                   7.81198(19)
_cell_length_c                   11.9892(3)
_cell_measurement_reflns_used    12224
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      35.381
_cell_measurement_theta_min      3.168
_cell_volume                     823.21(4)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      290(2)
_diffrn_detector_area_resol_mean 16.2711
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26379
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.998
_diffrn_reflns_theta_min         3.174
_exptl_absorpt_coefficient_mu    1.963
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[using a multifaceted crystal model (Clark & Reid, 1995)]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.1766
_exptl_crystal_size_mid          0.1165
_exptl_crystal_size_min          0.1115
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.571
_refine_ls_extinction_coef       0.0040(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL2013 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         3595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0178P)^2^+0.2170P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0479
_refine_ls_wR_factor_ref         0.0509
_reflns_number_gt                3077
_reflns_number_total             3595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm2775.cif
_cod_data_source_block           I
_cod_database_code               2238815
_shelx_hkl_checksum              46382
_shelx_res_checksum              50771
_shelxl_version_number           20.13