Palladium complexes containing novel cyclic selenium imides
Risto, Maarit; Eironen, Aino; Männistö, Elisa; Oilunkaniemi, Raija; Laitinen, Risto S.; Chivers, Tristram; Dalton Transactions  (2009) 8473–8475; doi:10.1039/b910049k

data_7002440
_publ_section_title
;
 Palladium complexes containing novel cyclic selenium imides
;
_journal_issue                   40
_journal_name_full               'Dalton Transactions'
_journal_page_first              8473
_journal_page_last               8475
_journal_paper_doi               10.1039/b910049k
_journal_year                    2009
_chemical_formula_moiety         'C12 H27 Cl2 N3 Pd Se4, C7 H5 N'
_chemical_formula_sum            'C19 H32 Cl2 N4 Pd Se4'
_chemical_formula_weight         809.63
_chemical_name_systematic
;

[tris(tert-butylimido)tetraselane)dichlorido-
palladium-benzonitrile(1/1)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.65(3)
_cell_angle_beta                 86.40(3)
_cell_angle_gamma                75.21(3)
_cell_formula_units_Z            2
_cell_length_a                   10.174(2)
_cell_length_b                   11.088(2)
_cell_length_c                   12.827(3)
_cell_measurement_reflns_used    5100
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.98
_cell_volume                     1327.7(6)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Branderburg & Berndt, 1999)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altonare, et al., 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker Nonius Kappaccd'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_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  0.0663
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19036
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    6.398
_exptl_absorpt_correction_T_max  0.5274
_exptl_absorpt_correction_T_min  0.2947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SHELXTL; Bruker 2001)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.950
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       0.0045(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0370P)^2^+8.5036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                4127
_reflns_number_total             5100
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b910049k.txt
_cod_data_source_block           cmpd2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7002440