#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/36/2233667.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_2233667
loop_
_publ_author_name
'Ha, Kwang'
_publ_section_title
;
 Bis(azido-κN)(1,10-phenanthroline-κ²N,N')palladium(II)
;
_journal_coeditor_code           WM2583
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m145
_journal_paper_doi               10.1107/S1600536812001201
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Pd (N3)2 (C12 H8 N2)]'
_chemical_formula_moiety         'C12 H8 N8 Pd'
_chemical_formula_sum            'C12 H8 N8 Pd'
_chemical_formula_weight         370.66
_chemical_name_systematic
;
Bis(azido-κN)(1,10-phenanthroline-κ²N,N')palladium(II)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.0724(3)
_cell_length_b                   18.3069(7)
_cell_length_c                   19.1309(7)
_cell_measurement_reflns_used    6741
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.47
_cell_volume                     2476.95(17)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'φ and ω 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  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17018
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.13
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.505
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.885891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.988
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.203
_refine_diff_density_min         -0.619
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0326
_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/[σ²(Fo²)+(0.0259P)²+3.9659P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0839
_reflns_number_gt                2244
_reflns_number_total             3058
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm2583.cif
_cod_data_source_block           global
_cod_database_code               2233667
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Pd Pd1 0.42841(4) 0.384720(15) 0.171291(14) 0.03115(10) Uani d . 1 1
N N1 0.3530(4) 0.48761(16) 0.20092(16) 0.0328(7) Uani d . 1 1
N N2 0.4398(4) 0.37116(16) 0.27707(15) 0.0322(7) Uani d . 1 1
N N3 0.4003(5) 0.41288(19) 0.07018(17) 0.0443(8) Uani d . 1 1
N N4 0.4887(5) 0.38609(18) 0.02351(18) 0.0408(8) Uani d . 1 1
N N5 0.5675(6) 0.3639(2) -0.02492(19) 0.0547(10) Uani d . 1 1
N N6 0.5003(6) 0.27920(19) 0.15822(18) 0.0463(9) Uani d . 1 1
N N7 0.5375(5) 0.25334(19) 0.10364(19) 0.0479(9) Uani d . 1 1
N N8 0.5816(8) 0.2236(2) 0.0529(2) 0.0781(15) Uani d . 1 1
C C1 0.3151(5) 0.5454(2) 0.1609(2) 0.0391(9) Uani d . 1 1
H H1 0.3208 0.5405 0.1115 0.047 Uiso calc R 1 1
C C2 0.2672(6) 0.6127(2) 0.1898(2) 0.0450(10) Uani d . 1 1
H H2 0.2401 0.6529 0.1600 0.054 Uiso calc R 1 1
C C3 0.2592(6) 0.6212(2) 0.2605(2) 0.0461(10) Uani d . 1 1
H H3 0.2269 0.6673 0.2800 0.055 Uiso calc R 1 1
C C4 0.2989(5) 0.5615(2) 0.3045(2) 0.0397(9) Uani d . 1 1
C C5 0.2938(6) 0.5635(2) 0.3793(2) 0.0465(10) Uani d . 1 1
H H5 0.2607 0.6076 0.4023 0.056 Uiso calc R 1 1
C C6 0.3351(6) 0.5037(2) 0.4177(2) 0.0472(10) Uani d . 1 1
H H6 0.3288 0.5068 0.4673 0.057 Uiso calc R 1 1
C C7 0.3880(5) 0.4360(2) 0.3861(2) 0.0391(9) Uani d . 1 1
C C8 0.4377(6) 0.3725(3) 0.4225(2) 0.0452(10) Uani d . 1 1
H H8 0.4366 0.3722 0.4721 0.054 Uiso calc R 1 1
C C9 0.4880(6) 0.3106(2) 0.3863(2) 0.0461(10) Uani d . 1 1
H H9 0.5228 0.2675 0.4107 0.055 Uiso calc R 1 1
C C10 0.4876(6) 0.3116(2) 0.3135(2) 0.0398(9) Uani d . 1 1
H H10 0.5223 0.2685 0.2889 0.048 Uiso calc R 1 1
C C11 0.3921(5) 0.4327(2) 0.31269(19) 0.0330(8) Uani d . 1 1
C C12 0.3466(5) 0.49549(19) 0.27182(19) 0.0330(8) Uani d . 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 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
_geom_angle_publ_flag
N1 Pd1 N2 81.20(12) y
N3 Pd1 N6 98.71(14) y
N3 Pd1 N1 90.27(13) ?
N6 Pd1 N1 170.93(13) ?
N3 Pd1 N2 171.39(13) ?
N6 Pd1 N2 89.80(13) ?
C1 N1 C12 118.7(3) ?
C1 N1 Pd1 128.8(3) ?
C12 N1 Pd1 112.5(2) ?
C10 N2 C11 118.5(3) ?
C10 N2 Pd1 128.8(3) ?
C11 N2 Pd1 112.7(2) ?
N4 N3 Pd1 124.1(3) ?
N5 N4 N3 174.8(4) ?
N7 N6 Pd1 123.6(3) ?
N8 N7 N6 174.5(5) ?
N1 C1 C2 121.6(4) ?
N1 C1 H1 119.2 ?
C2 C1 H1 119.2 ?
C3 C2 C1 120.3(4) ?
C3 C2 H2 119.9 ?
C1 C2 H2 119.9 ?
C2 C3 C4 119.8(4) ?
C2 C3 H3 120.1 ?
C4 C3 H3 120.1 ?
C12 C4 C3 116.8(4) ?
C12 C4 C5 118.2(4) ?
C3 C4 C5 125.0(4) ?
C6 C5 C4 121.3(4) ?
C6 C5 H5 119.4 ?
C4 C5 H5 119.4 ?
C5 C6 C7 121.9(4) ?
C5 C6 H6 119.0 ?
C7 C6 H6 119.0 ?
C8 C7 C11 117.1(4) ?
C8 C7 C6 125.2(4) ?
C11 C7 C6 117.7(4) ?
C9 C8 C7 120.0(4) ?
C9 C8 H8 120.0 ?
C7 C8 H8 120.0 ?
C8 C9 C10 119.5(4) ?
C8 C9 H9 120.2 ?
C10 C9 H9 120.2 ?
N2 C10 C9 122.1(4) ?
N2 C10 H10 118.9 ?
C9 C10 H10 118.9 ?
N2 C11 C7 122.7(3) ?
N2 C11 C12 116.7(3) ?
C7 C11 C12 120.6(4) ?
N1 C12 C4 122.8(3) ?
N1 C12 C11 116.9(3) ?
C4 C12 C11 120.3(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 N1 2.038(3) y
Pd1 N2 2.040(3) y
Pd1 N3 2.012(3) y
Pd1 N6 2.013(3) y
N1 C1 1.333(5) ?
N1 C12 1.365(5) ?
N2 C10 1.338(5) ?
N2 C11 1.360(5) ?
N3 N4 1.195(5) ?
N4 N5 1.155(5) ?
N6 N7 1.176(5) ?
N7 N8 1.156(5) ?
C1 C2 1.392(5) ?
C1 H1 0.9500 ?
C2 C3 1.363(6) ?
C2 H2 0.9500 ?
C3 C4 1.407(6) ?
C3 H3 0.9500 ?
C4 C12 1.402(5) ?
C4 C5 1.432(6) ?
C5 C6 1.350(6) ?
C5 H5 0.9500 ?
C6 C7 1.430(6) ?
C6 H6 0.9500 ?
C7 C8 1.399(6) ?
C7 C11 1.407(5) ?
C8 C9 1.374(6) ?
C8 H8 0.9500 ?
C9 C10 1.392(5) ?
C9 H9 0.9500 ?
C10 H10 0.9500 ?
C11 C12 1.427(5) ?
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
C1 H1 N3 . 0.95 2.53 3.044(5) 114.0
C1 H1 N5 5_665 0.95 2.54 3.196(5) 126.8
C5 H5 N8 3_655 0.95 2.55 3.324(6) 139.3
C8 H8 N8 7_566 0.95 2.55 3.218(6) 127.4
C10 H10 N6 . 0.95 2.51 3.031(5) 114.3
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N3 Pd1 N1 C1 -3.1(3)
N2 Pd1 N1 C1 178.1(3)
N3 Pd1 N1 C12 178.3(3)
N2 Pd1 N1 C12 -0.5(2)
N6 Pd1 N2 C10 2.4(3)
N1 Pd1 N2 C10 -178.7(3)
N6 Pd1 N2 C11 -178.0(3)
N1 Pd1 N2 C11 0.9(2)
N6 Pd1 N3 N4 -30.7(4)
N3 Pd1 N6 N7 9.6(4)
N2 Pd1 N6 N7 -171.7(4)
C12 N1 C1 C2 -0.8(5)
Pd1 N1 C1 C2 -179.3(3)
N1 C1 C2 C3 0.4(6)
C1 C2 C3 C4 -0.2(6)
C2 C3 C4 C12 0.4(6)
C2 C3 C4 C5 -179.5(4)
C12 C4 C5 C6 0.5(6)
C3 C4 C5 C6 -179.6(4)
C4 C5 C6 C7 0.8(6)
C5 C6 C7 C8 178.1(4)
C5 C6 C7 C11 -1.3(6)
C11 C7 C8 C9 0.1(6)
C6 C7 C8 C9 -179.3(4)
C7 C8 C9 C10 -0.5(6)
C11 N2 C10 C9 0.6(6)
Pd1 N2 C10 C9 -179.8(3)
C8 C9 C10 N2 0.1(6)
C10 N2 C11 C7 -1.0(5)
Pd1 N2 C11 C7 179.3(3)
C10 N2 C11 C12 178.5(3)
Pd1 N2 C11 C12 -1.2(4)
C8 C7 C11 N2 0.6(5)
C6 C7 C11 N2 -179.9(3)
C8 C7 C11 C12 -178.9(3)
C6 C7 C11 C12 0.6(5)
C1 N1 C12 C4 1.0(5)
Pd1 N1 C12 C4 179.7(3)
C1 N1 C12 C11 -178.7(3)
Pd1 N1 C12 C11 0.0(4)
C3 C4 C12 N1 -0.8(6)
C5 C4 C12 N1 179.1(3)
C3 C4 C12 C11 178.9(3)
C5 C4 C12 C11 -1.2(5)
N2 C11 C12 N1 0.8(5)
C7 C11 C12 N1 -179.7(3)
N2 C11 C12 C4 -178.9(3)
C7 C11 C12 C4 0.6(5)
