#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:29:14 +0100 (jue 24 de mar de 2016) $
#$Revision: 179581 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/46/4504609.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_4504609
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 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 101.147(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.2650(9)
_cell_length_b                   7.5468(7)
_cell_length_c                   9.9279(9)
_cell_measurement_reflns_used    106
_cell_measurement_temperature    173(2)
_cell_volume                     754.58(12)
_computing_cell_refinement       'SMART (Siemens, 1995b)'
_computing_data_collection       'SMART (Siemens, 1995b)'
_computing_data_reduction        'SMART (Siemens, 1995b)'
_computing_molecular_graphics    'SMART (Siemens, 1995a)'
_computing_publication_material  'SMART (Siemens, 1995a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow 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  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4728
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.919
_exptl_absorpt_correction_T_max  0.646826
_exptl_absorpt_correction_T_min  0.487340
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.842
_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          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.0196(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         1736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0178
_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)+(0.0207P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0425
_refine_ls_wR_factor_ref         0.0428
_reflns_number_gt                1522
_reflns_number_total             1736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg050362osi20050725_015150.cif
_cod_data_source_block           14b
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4504609
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 -1.0000 0.0000 0.01548(8) Uani 1 2 d S
Cl1 Cl 0.02160(4) -0.83911(6) -0.19266(5) 0.02102(12) Uani 1 1 d .
Cl2 Cl -0.22817(4) -0.98161(6) -0.06375(5) 0.02221(11) Uani 1 1 d .
N1 N 0.21926(15) -1.0698(2) -0.33104(16) 0.0204(4) Uani 1 1 d .
H10A H 0.1535 -1.0406 -0.2870 0.025 Uiso 1 1 calc R
H10B H 0.2196 -1.1884 -0.3400 0.025 Uiso 1 1 calc R
C3 C 0.44307(18) -0.9729(2) -0.46320(19) 0.0179(4) Uani 1 1 d .
H3A H 0.4456 -0.8439 -0.4513 0.021 Uiso 1 1 calc R
C1 C 0.3478(2) -1.0115(3) -0.2484(2) 0.0242(4) Uani 1 1 d .
H1A H 0.3619 -1.0682 -0.1591 0.029 Uiso 1 1 calc R
H1B H 0.3463 -0.8844 -0.2346 0.029 Uiso 1 1 calc R
C5 C 0.19336(19) -0.9862(3) -0.4706(2) 0.0239(4) Uani 1 1 d .
H5A H 0.1835 -0.8592 -0.4615 0.029 Uiso 1 1 calc R
H5B H 0.1111 -1.0323 -0.5238 0.029 Uiso 1 1 calc R
C4 C 0.30658(19) -1.0239(3) -0.5455(2) 0.0217(4) Uani 1 1 d .
H4A H 0.2908 -0.9592 -0.6316 0.026 Uiso 1 1 calc R
H4B H 0.3067 -1.1493 -0.5671 0.026 Uiso 1 1 calc R
C2 C 0.46065(19) -1.0592(3) -0.3206(2) 0.0222(4) Uani 1 1 d .
H2A H 0.4644 -1.1869 -0.3303 0.027 Uiso 1 1 calc R
H2B H 0.5441 -1.0205 -0.2650 0.027 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 0.01390(11) 0.01630(11) 0.01692(12) 0.00018(8) 0.00465(8) 0.00171(8)
Cl1 0.0210(2) 0.0227(2) 0.0213(2) 0.00328(18) 0.00887(18) 0.00479(18)
Cl2 0.0154(2) 0.0261(3) 0.0252(3) 0.00398(19) 0.00423(19) 0.00170(18)
N1 0.0165(8) 0.0196(8) 0.0281(9) -0.0013(7) 0.0117(7) -0.0008(6)
C3 0.0140(9) 0.0198(10) 0.0214(10) -0.0003(7) 0.0075(8) -0.0002(7)
C1 0.0229(10) 0.0326(11) 0.0195(10) -0.0036(9) 0.0099(8) -0.0078(9)
C5 0.0140(9) 0.0303(11) 0.0283(11) 0.0038(9) 0.0064(8) 0.0024(8)
C4 0.0144(9) 0.0301(11) 0.0214(10) 0.0018(8) 0.0057(8) 0.0003(8)
C2 0.0139(10) 0.0329(11) 0.0205(10) 0.0008(8) 0.0052(8) -0.0018(8)
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_535
Cl2 Pd1 Cl1 90.223(16) . 3_535
Cl2 Pd1 Cl1 89.778(16) 3_535 3_535
Cl2 Pd1 Cl1 89.777(16) . .
Cl2 Pd1 Cl1 90.222(16) 3_535 .
Cl1 Pd1 Cl1 180.0 3_535 .
C1 N1 C5 111.56(15) . .
C4 C3 C2 108.55(15) . .
C4 C3 C3 112.24(19) . 3_634
C2 C3 C3 110.96(19) . 3_634
N1 C1 C2 110.34(16) . .
N1 C5 C4 110.95(16) . .
C5 C4 C3 113.50(16) . .
C1 C2 C3 111.73(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 Cl2 2.3092(5) .
Pd1 Cl2 2.3092(5) 3_535
Pd1 Cl1 2.3122(5) 3_535
Pd1 Cl1 2.3122(5) .
N1 C1 1.480(2) .
N1 C5 1.498(3) .
C3 C4 1.529(3) .
C3 C2 1.537(3) .
C3 C3 1.548(3) 3_634
C1 C2 1.519(3) .
C5 C4 1.523(2) .
