#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:29:14 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179581 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/46/4504608.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4504608
loop_
_publ_author_name
'Adams, Christopher J.'
'Angeloni, Alessandro'
'Orpen, A. Guy'
'Podesta, Thomas J.'
'Shore, Benjamin'
_publ_section_title
;
 Crystal Synthesis of Organic−Inorganic Hybrid Salts Based on
 Tetrachloroplatinate and -palladate Salts of Organic Cations: 
 Formation of Linear, Two-, and Three-Dimensional
 NH···Cl Hydrogen Bond Networks
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              411
_journal_paper_doi               10.1021/cg050362o
_journal_volume                  6
_journal_year                    2006
_chemical_formula_sum            'C10 H22 Cl4 N2 Pd'
_chemical_formula_weight         418.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.736(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.9658(12)
_cell_length_b                   10.7111(17)
_cell_length_c                   11.6778(31)
_cell_measurement_reflns_used    99
_cell_measurement_temperature    173(2)
_cell_volume                     742.5(3)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Bruker Shelxtl'
_computing_publication_material  'Bruker xcif'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker area detector'
_diffrn_measurement_method       'omega frames'
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4723
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.950
_exptl_absorpt_correction_T_max  0.694161
_exptl_absorpt_correction_T_min  0.542802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 G. M. Sheldrick. 
 SADABS: A program for absorption correction with the Siemens SMART system; 
 University of Göttingen: Germany, 1996.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.0022(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         1699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0212
_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)+(0.0303P)²+0.3478P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0571
_reflns_number_gt                1549
_reflns_number_total             1699
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg050362osi20050725_015150.cif
_cod_data_source_block           14a
_cod_original_cell_volume        742.48(23)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4504608
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_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
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd 0.0000 0.5000 0.0000 0.01524(9) Uani 1 2 d S
Cl1 Cl 0.11878(8) 0.35473(4) 0.13875(4) 0.02101(12) Uani 1 1 d .
Cl2 Cl 0.28754(9) 0.63259(5) 0.06435(5) 0.03325(15) Uani 1 1 d .
C1 C 0.9237(3) -0.0934(2) 0.16758(17) 0.0213(4) Uani 1 1 d .
H1A H 0.9900 -0.1737 0.1894 0.026 Uiso 1 1 calc R
H1B H 1.0366 -0.0436 0.1344 0.026 Uiso 1 1 calc R
C2 C 0.7219(3) -0.11214(18) 0.07913(17) 0.0207(4) Uani 1 1 d .
H2A H 0.6144 -0.1667 0.1111 0.025 Uiso 1 1 calc R
H2B H 0.7710 -0.1529 0.0118 0.025 Uiso 1 1 calc R
C3 C 0.6054(3) 0.01086(16) 0.04265(16) 0.0158(4) Uani 1 1 d .
H3A H 0.7117 0.0619 0.0042 0.019 Uiso 1 1 calc R
C4 C 0.5472(3) 0.08113(19) 0.15056(16) 0.0193(4) Uani 1 1 d .
H4A H 0.4911 0.1635 0.1282 0.023 Uiso 1 1 calc R
H4B H 0.4278 0.0368 0.1840 0.023 Uiso 1 1 calc R
C5 C 0.7479(4) 0.09480(18) 0.24120(17) 0.0211(4) Uani 1 1 d .
H5A H 0.8591 0.1493 0.2122 0.025 Uiso 1 1 calc R
H5B H 0.6987 0.1329 0.3098 0.025 Uiso 1 1 calc R
N1 N 0.8528(3) -0.02929(17) 0.27148(14) 0.0188(3) Uani 1 1 d .
H2N H 0.9736 -0.0185 0.3232 0.023 Uiso 1 1 calc R
H1N H 0.7532 -0.0776 0.3040 0.023 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.01435(13) 0.01801(13) 0.01292(12) -0.00069(7) -0.00078(7) 0.00001(7)
Cl1 0.0226(2) 0.0220(2) 0.0176(2) 0.00212(17) -0.00168(17) 0.00246(18)
Cl2 0.0285(3) 0.0258(3) 0.0413(3) 0.0061(2) -0.0167(2) -0.0083(2)
C1 0.0182(9) 0.0266(10) 0.0188(9) -0.0027(8) -0.0001(7) 0.0033(8)
C2 0.0199(10) 0.0224(10) 0.0185(9) -0.0034(7) -0.0042(7) 0.0035(8)
C3 0.0168(9) 0.0179(9) 0.0122(9) -0.0003(6) -0.0010(7) -0.0020(7)
C4 0.0206(10) 0.0198(9) 0.0167(9) -0.0024(7) -0.0026(7) 0.0028(7)
C5 0.0256(10) 0.0191(9) 0.0176(9) -0.0019(7) -0.0027(7) -0.0003(8)
N1 0.0175(8) 0.0235(8) 0.0144(8) 0.0005(6) -0.0033(6) -0.0022(7)
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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
Cl2 Pd1 Cl2 180.0 . 3_565
Cl2 Pd1 Cl1 88.833(18) . 3_565
Cl2 Pd1 Cl1 91.168(19) 3_565 3_565
Cl2 Pd1 Cl1 91.167(18) . .
Cl2 Pd1 Cl1 88.833(18) 3_565 .
Cl1 Pd1 Cl1 180.0 3_565 .
N1 C1 C2 110.12(16) . .
C1 C2 C3 112.50(16) . .
C2 C3 C4 109.08(15) . .
C2 C3 C3 111.62(18) . 3_655
C4 C3 C3 111.5(2) . 3_655
C5 C4 C3 112.98(16) . .
N1 C5 C4 111.09(15) . .
C1 N1 C5 111.26(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 Cl2 2.2949(5) .
Pd1 Cl2 2.2949(5) 3_565
Pd1 Cl1 2.3063(5) 3_565
Pd1 Cl1 2.3063(5) .
C1 N1 1.492(3) .
C1 C2 1.519(3) .
C2 C3 1.530(3) .
C3 C4 1.537(3) .
C3 C3 1.542(4) 3_655
C4 C5 1.524(3) .
C5 N1 1.496(3) .
