#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/59/2235918.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_2235918
loop_
_publ_author_name
'Abellán-López, Antonio'
'Chicote-Olalla, María Teresa'
'Bautista-Cerezo, Delia'
_publ_section_title
;
 cis-Diiodido(N,N,N',N'-tetramethylethylenediamine-κ²N,N')palladium(II)
;
_journal_coeditor_code           LR2073
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1129
_journal_paper_doi               10.1107/S1600536812033004
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Pd I2 (C6 H16 N2)]'
_chemical_formula_moiety         'C6 H16 I2 N2  Pd'
_chemical_formula_sum            'C6 H16 I2 N2 Pd'
_chemical_formula_weight         476.41
_chemical_name_systematic
;
cis-Diiodido(N,N,N',N'-\
tetramethylethylenediamine-κ²N,N')palladium(II)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 107.262(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9266(4)
_cell_length_b                   14.6911(7)
_cell_length_c                   10.5309(5)
_cell_measurement_reflns_used    4971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.05
_cell_measurement_theta_min      2.77
_cell_volume                     1171.09(10)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω scan'
_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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0153
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6502
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.05
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    6.810
_exptl_absorpt_correction_T_max  0.8218
_exptl_absorpt_correction_T_min  0.5811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.229
_refine_diff_density_min         -0.727
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         1351
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0232
_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)+(0.0250P)²+10.9315P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0597
_reflns_number_gt                1326
_reflns_number_total             1351
_reflns_threshold_expression     I>2sigma(I)
_iucr_refine_instructions_details
;
TITL aa342s in C2/c
CELL 0.71073   7.9266  14.6911  10.5309  90.000 107.262  90.000
ZERR    4.00   0.0004   0.0007   0.0005   0.000   0.002   0.000
LATT 7
SYMM -X, Y, 0.5-Z
SFAC C  H  N  O  Pd I
UNIT 24 64 8 0  4 8
omit -2   2   1
omit -4   2   5
omit   -1   7   4
omit    3   1   0
omit -4   6   2
omit 3   1   1
omit -3   3   1
omit 0   2   2
omit 1   1   4
omit 0   0   4
omit 3   5   1
conf
bond $h
eqiv $1 1-x, y, 0.5-z
conf n1 c1 C1_$1 n1_$1
mpla n1 c2 c3
mpla n1_$1  c2_$1  c3_$1
mpla pd1 n1 I1 n1_$1 I1_$1
L.S. 20
acta 52
size 0.22    0.15  0.03
FMAP 2
PLAN 10
TEMP -173
WGHT    0.025000   10.931499
FVAR       0.22570
PD1   5    0.500000    0.517981    0.250000    10.50000    0.01163    0.01133 =
         0.00958    0.00000    0.00366    0.00000
I1    6    0.711541    0.644568    0.373844    11.00000    0.02803    0.02164 =
         0.01984   -0.00239    0.00561   -0.01018
N1    3    0.331732    0.411056    0.150405    11.00000    0.01237    0.01688 =
         0.01192   -0.00280    0.00401   -0.00166
C1    1    0.442675    0.327523    0.179445    11.00000    0.02141    0.01404 =
         0.02239   -0.00382    0.00731   -0.00036
AFIX  23
H1A   2    0.517533    0.324604    0.119186    11.00000   -1.20000
H1B   2    0.365613    0.273080    0.163167    11.00000   -1.20000
AFIX   0
C2    1    0.180729    0.403472    0.205725    11.00000    0.01451    0.02911 =
         0.02150   -0.00343    0.00904   -0.00520
AFIX 137
H2A   2    0.112874    0.460279    0.189579    11.00000   -1.50000
H2B   2    0.225052    0.392188    0.301632    11.00000   -1.50000
H2C   2    0.104453    0.352938    0.162530    11.00000   -1.50000
AFIX   0
C3    1    0.260538    0.420522    0.003833    11.00000    0.02447    0.02543 =
         0.01345   -0.00426    0.00333   -0.00458
AFIX 137
H3A   2    0.194669    0.365445   -0.033564    11.00000   -1.50000
H3B   2    0.358352    0.429051   -0.034113    11.00000   -1.50000
H3C   2    0.181590    0.473321   -0.017594    11.00000   -1.50000
HKLF 4
;
_cod_data_source_file            lr2073.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2235918
_cod_database_fobs_code          2235918
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Pd Pd1 0.5000 0.51798(3) 0.2500 0.01073(10) Uani d S 1 2
I I1 0.71154(4) 0.644568(18) 0.37384(3) 0.02349(10) Uani d . 1 1
N N1 0.3317(4) 0.4111(2) 0.1504(3) 0.0136(6) Uani d . 1 1
C C1 0.4427(5) 0.3275(3) 0.1794(4) 0.0191(8) Uani d . 1 1
H H1A 0.5175 0.3246 0.1192 0.023 Uiso calc R 1 1
H H1B 0.3656 0.2731 0.1632 0.023 Uiso calc R 1 1
C C2 0.1807(5) 0.4035(3) 0.2057(4) 0.0209(8) Uani d . 1 1
H H2A 0.1129 0.4603 0.1896 0.031 Uiso calc R 1 1
H H2B 0.2251 0.3922 0.3016 0.031 Uiso calc R 1 1
H H2C 0.1045 0.3529 0.1625 0.031 Uiso calc R 1 1
C C3 0.2605(6) 0.4205(3) 0.0038(4) 0.0216(8) Uani d . 1 1
H H3A 0.1947 0.3654 -0.0336 0.032 Uiso calc R 1 1
H H3B 0.3584 0.4291 -0.0341 0.032 Uiso calc R 1 1
H H3C 0.1816 0.4733 -0.0176 0.032 Uiso calc R 1 1
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 0.01163(18) 0.01133(18) 0.00958(18) 0.000 0.00366(13) 0.000
I1 0.02803(17) 0.02164(16) 0.01984(16) -0.01018(10) 0.00561(11) -0.00239(10)
N1 0.0124(14) 0.0169(15) 0.0119(14) -0.0017(12) 0.0040(11) -0.0028(12)
C1 0.0214(19) 0.0140(17) 0.022(2) -0.0004(15) 0.0073(16) -0.0038(15)
C2 0.0145(18) 0.029(2) 0.022(2) -0.0052(15) 0.0090(15) -0.0034(17)
C3 0.024(2) 0.025(2) 0.0134(18) -0.0046(16) 0.0033(15) -0.0043(16)
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'
O O 0.0106 0.0060 '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'
I I -0.4742 1.8119 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 Pd1 N1 . 2_655 84.68(18)
N1 Pd1 I1 . . 178.36(9)
N1 Pd1 I1 2_655 . 93.71(9)
N1 Pd1 I1 . 2_655 93.71(9)
N1 Pd1 I1 2_655 2_655 178.36(9)
I1 Pd1 I1 . 2_655 87.906(18)
C2 N1 C3 . . 108.3(3)
C2 N1 C1 . . 110.7(3)
C3 N1 C1 . . 108.1(3)
C2 N1 Pd1 . . 108.9(2)
C3 N1 Pd1 . . 115.7(2)
C1 N1 Pd1 . . 105.2(2)
N1 C1 C1 . 2_655 110.6(3)
N1 C1 H1A . . 109.5
C1 C1 H1A 2_655 . 109.5
N1 C1 H1B . . 109.5
C1 C1 H1B 2_655 . 109.5
H1A C1 H1B . . 108.1
N1 C2 H2A . . 109.5
N1 C2 H2B . . 109.5
H2A C2 H2B . . 109.5
N1 C2 H2C . . 109.5
H2A C2 H2C . . 109.5
H2B C2 H2C . . 109.5
N1 C3 H3A . . 109.5
N1 C3 H3B . . 109.5
H3A C3 H3B . . 109.5
N1 C3 H3C . . 109.5
H3A C3 H3C . . 109.5
H3B C3 H3C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Pd1 N1 . 2.125(3)
Pd1 N1 2_655 2.125(3)
Pd1 I1 . 2.5833(4)
Pd1 I1 2_655 2.5833(4)
N1 C2 . 1.483(5)
N1 C3 . 1.484(5)
N1 C1 . 1.488(5)
C1 C1 2_655 1.494(8)
C1 H1A . 0.9900
C1 H1B . 0.9900
C2 H2A . 0.9800
C2 H2B . 0.9800
C2 H2C . 0.9800
C3 H3A . 0.9800
C3 H3B . 0.9800
C3 H3C . 0.9800
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_site_symmetry_1
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
N1 Pd1 N1 C2 2_655 . . 104.9(3)
I1 Pd1 N1 C2 2_655 . . -74.8(2)
N1 Pd1 N1 C3 2_655 . . -133.0(3)
I1 Pd1 N1 C3 2_655 . . 47.3(3)
N1 Pd1 N1 C1 2_655 . . -13.83(18)
I1 Pd1 N1 C1 2_655 . . 166.5(2)
C2 N1 C1 C1 . . 2_655 -77.3(4)
C3 N1 C1 C1 . . 2_655 164.2(4)
Pd1 N1 C1 C1 . . 2_655 40.1(4)
N1 C1 C1 N1 . 2_655 2_655 -56.4(6)
