Coordination of bis(pyrazol-1-yl)amine to palladium(II): influence of the co-ligands and counter-ions on the molecular and crystal structures
Mendoza, María de los Angeles; Bernès, Sylvain; Mendoza-Díaz, Guillermo; Acta Crystallographica Section E 71 (2015) 22–27; doi:10.1107/S205698901402595X

data_2240283
_publ_section_title
;
 Coordination of bis(pyrazol-1-yl)amine to palladium(II): influence of the
 co-ligands and counter-ions on the molecular and crystal structures
;
_journal_coeditor_code           WM5076
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              22
_journal_page_last               27
_journal_paper_doi               10.1107/S205698901402595X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Pd I (C14 H2 N5)] I, 0.5H2 O'
_chemical_formula_moiety         'C14 H23 I N5 Pd +, I -, 0.5(H2 O)'
_chemical_formula_sum            'C14 H24 I2 N5 O0.5 Pd'
_chemical_formula_weight         630.58
_chemical_name_systematic
'{Bis[2-(3,5-dimethylpyrazol-1-yl-\k<i>N</i>^2^)ethyl]amine-\k<i>N</i>}iodidopalladium iodide hemihydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
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_cell_angle_alpha                106.17(2)
_cell_angle_beta                 97.34(3)
_cell_angle_gamma                106.79(3)
_cell_formula_units_Z            4
_cell_length_a                   12.013(4)
_cell_length_b                   12.089(4)
_cell_length_c                   15.162(5)
_cell_measurement_reflns_used    68
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      12.04
_cell_measurement_theta_min      4.24
_cell_volume                     1972.1(13)
_computing_cell_refinement
;
XSCANS (Siemens, 1996)
;
_computing_data_collection
;
XSCANS (Siemens, 1996)
;
_computing_data_reduction
;
XSCANS (Siemens, 1996)
;
_computing_molecular_graphics
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SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
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SHELXTL (Sheldrick, 2008)
;
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SHELXL2014 (Sheldrick, 2008)
;
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;
SHELXS2014 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\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  0.0427
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         1.818
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
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_exptl_absorpt_correction_T_max  0.523
_exptl_absorpt_correction_T_min  0.446
_exptl_absorpt_correction_type   psi-scan
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;
(XSCANS; Siemens, 1996)
;
_exptl_crystal_colour            Orange
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_exptl_crystal_description       Plate
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_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
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_refine_diff_density_min         -1.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         6835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0324P)^2^+6.3989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.1012
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_reflns_threshold_expression     I>2\s(I)
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_cod_data_source_block           3
_cod_original_cell_volume        1972.0(11)
_cod_original_formula_sum        'C14 H24 I2 N5 O0.50 Pd'
_cod_database_code               2240283
_cod_database_fobs_code          2240283
_shelx_hkl_checksum              8253
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