#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/88/2208816.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2208816
loop_
_publ_author_name
'Ademi, Lumni'
'Constable, Edwin C.'
'Housecroft, Catherine E.'
'Neuburger, Markus'
'Schaffner, Silvia'
_publ_section_title
;
 trans-Diacetonitriledibromopalladium(II)
;
_journal_coeditor_code           CF2021
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1059
_journal_page_last               m1061
_journal_paper_doi               10.1107/S1600536806013377
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Pd1 Br2 (C2 H3 N1)2]'
_chemical_formula_moiety         'C4 H6 Br2 N2 Pd1'
_chemical_formula_sum            'C4 H6 Br2 N2 Pd'
_chemical_formula_weight         348.31
_chemical_name_systematic
;
trans-Diacetonitriledibromopalladium(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90.327(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.1979(3)
_cell_length_b                   12.0686(7)
_cell_length_c                   7.0740(3)
_cell_measurement_reflns_used    2403
_cell_measurement_temperature    173
_cell_measurement_theta_max      30
_cell_measurement_theta_min      1
_cell_volume                     443.75(4)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001)'
_computing_data_reduction        DENZO/SCALEPACK
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge et al.,  2003)'
_computing_structure_solution    'SIR92 (Altomare et al.,  1994)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4797
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         3.338
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.019
_exptl_absorpt_correction_T_max  0.19
_exptl_absorpt_correction_T_min  0.10
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    2.607
_exptl_crystal_description       block
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.67
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0304
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         1003
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.0
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
w = [1-(Fₒ-Fc)²/36σ²(F)]²/[0.377T₀(x)+0.221T₁(x)+0.171T₂(x)]
where Ti are Chebychev polynomials and x = Fc/Fₘₐₓ
(Prince, 1982; Watkin, 1994)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0320
_refine_ls_wR_factor_gt          0.0246
_refine_ls_wR_factor_ref         0.0246
_reflns_number_gt                1003
_reflns_number_total             1291
_reflns_threshold_expression     I>3σ(I)
_cod_data_source_file            cf2021.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C4 H6 Br2 N2 Pd1'
_cod_database_code               2208816
_cod_database_fobs_code          2208816
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
Pd Pd1 0.0000 0.0000 0.0000 0.0244 Uani 1.0000
Br Br1 0.11120(6) 0.13106(2) -0.24527(4) 0.0350 Uani 1.0000
C C1 0.4168(5) 0.1036(2) 0.2610(4) 0.0290 Uani 1.0000
C C2 0.6111(6) 0.1530(3) 0.3828(4) 0.0356 Uani 1.0000
N N1 0.2656(4) 0.0645(2) 0.1656(3) 0.0301 Uani 1.0000
H H21 0.5299 0.1978 0.4771 0.0442 Uiso 1.0000
H H22 0.7025 0.0919 0.4429 0.0439 Uiso 1.0000
H H23 0.7360 0.1958 0.3147 0.0437 Uiso 1.0000
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pd1 0.02135(13) 0.02418(14) 0.02775(14) 0.00090(9) -0.00431(9) -0.00419(11)
Br1 0.03403(16) 0.03435(16) 0.03645(16) -0.00327(11) -0.00444(11) 0.00418(12)
C1 0.0262(12) 0.0313(12) 0.0295(12) 0.0019(10) -0.0010(10) 0.0007(10)
C2 0.0296(13) 0.0401(15) 0.0372(14) -0.0046(12) -0.0061(11) -0.0082(12)
N1 0.0275(10) 0.0303(11) 0.0322(11) 0.0001(9) -0.0063(8) -0.0031(9)
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0033 0.0016 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Br -0.2901 2.4595 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Br1 Pd1 N1 2_555 2_555 89.93(7) no
Br1 Pd1 Br1 2_555 . 180 no
N1 Pd1 Br1 2_555 . 90.07(7) no
Br1 Pd1 N1 2_555 . 90.07(7) no
N1 Pd1 N1 2_555 . 180 no
Br1 Pd1 N1 . . 89.93(7) yes
C2 C1 N1 . . 179.6(3) yes
C1 C2 H21 . . 109.7 no
C1 C2 H22 . . 106.5 no
H21 C2 H22 . . 109.8 no
C1 C2 H23 . . 113.1 no
H21 C2 H23 . . 110.2 no
H22 C2 H23 . . 107.3 no
Pd1 N1 C1 . . 178.7(2) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 Br1 2_555 2.4203(3) no
Pd1 N1 2_555 1.966(2) no
Pd1 Br1 . 2.4203(3) yes
Pd1 N1 . 1.966(2) yes
C1 C2 . 1.452(4) yes
C1 N1 . 1.136(4) yes
C2 H21 . 0.959 no
C2 H22 . 0.974 no
C2 H23 . 0.962 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C2 H21 Br1 1_556 0.96 3.05 3.718(3) 128 yes
C2 H22 Br1 1_656 0.97 3.09 3.698(3) 122 yes
C2 H23 Br1 4_655 0.96 2.89 3.794(3) 157 yes
