#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:02:21 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179948 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/43/7024396.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_7024396
loop_
_publ_author_name
'Khalaf, Majid S.'
'Oakley, Sarah H.'
'Coles, Martyn P.'
'Hitchcock, Peter B.'
_publ_section_title
;
 Coordination of neutral, methylene bridged bis-guanidyls at palladium.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1635
_journal_page_last               1642
_journal_paper_doi               10.1039/b916520g
_journal_volume                  39
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C16 H29 Cl N6 Pd'
_chemical_formula_sum            'C16 H29 Cl N6 Pd'
_chemical_formula_weight         447.3
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2004-11-10T15:25:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9381(3)
_cell_length_b                   11.6842(4)
_cell_length_c                   14.1258(5)
_cell_measurement_reflns_used    26957
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     1805.32(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.775756E-1
_diffrn_orient_matrix_UB_12      0.12681E-2
_diffrn_orient_matrix_UB_13      0.37445E-1
_diffrn_orient_matrix_UB_21      -0.48359E-1
_diffrn_orient_matrix_UB_22      -0.2782E-3
_diffrn_orient_matrix_UB_23      0.600776E-1
_diffrn_orient_matrix_UB_31      0.13068E-2
_diffrn_orient_matrix_UB_32      -0.855758E-1
_diffrn_orient_matrix_UB_33      0.3595E-3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28540
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         3.43
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.187
_exptl_absorpt_correction_T_max  1.0304
_exptl_absorpt_correction_T_min  0.8939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.034
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0231P)²+1.7753P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0657
_reflns_number_gt                3221
_reflns_number_total             3570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b916520g.txt
_cod_data_source_block           (1)-nov604
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7024396
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -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
Pd Pd 0.19281(3) 0.71577(2) 0.24045(2) 0.01952(9) Uani 1 1 d .
Cl Cl 0.38050(9) 0.80698(9) 0.23709(9) 0.0364(3) Uani 1 1 d .
N1 N 0.2422(3) 0.6054(3) 0.1239(2) 0.0212(8) Uani 1 1 d .
N2 N 0.0576(3) 0.6072(3) 0.0391(2) 0.0205(8) Uani 1 1 d .
N3 N 0.1908(4) 0.4513(3) 0.0257(2) 0.0249(8) Uani 1 1 d .
N4 N -0.0820(3) 0.7149(3) 0.1407(2) 0.0207(7) Uani 1 1 d .
N5 N 0.0327(2) 0.6245(2) 0.2569(3) 0.0185(7) Uani 1 1 d .
N6 N -0.1811(3) 0.6155(2) 0.2616(2) 0.0216(7) Uani 1 1 d .
C1 C 0.1655(4) 0.5548(4) 0.0657(3) 0.0212(10) Uani 1 1 d .
C2 C -0.0307(4) 0.5481(4) -0.0215(3) 0.0270(10) Uani 1 1 d .
H2A H -0.0868 0.6044 -0.0507 0.032 Uiso 1 1 calc R
H2B H -0.08 0.4942 0.0169 0.032 Uiso 1 1 calc R
C3 C 0.0371(4) 0.4836(4) -0.0975(3) 0.0312(12) Uani 1 1 d .
H3A H -0.0215 0.444 -0.1397 0.037 Uiso 1 1 calc R
H3B H 0.0865 0.5371 -0.1362 0.037 Uiso 1 1 calc R
C4 C 0.1186(4) 0.3982(4) -0.0495(3) 0.0310(11) Uani 1 1 d .
H4A H 0.068 0.3361 -0.0223 0.037 Uiso 1 1 calc R
H4B H 0.1743 0.3637 -0.0968 0.037 Uiso 1 1 calc R
C5 C 0.2720(4) 0.3703(4) 0.0735(4) 0.0368(12) Uani 1 1 d .
H5A H 0.3329 0.3412 0.0276 0.044 Uiso 1 1 calc R
H5B H 0.2234 0.3043 0.0962 0.044 Uiso 1 1 calc R
C6 C 0.3375(4) 0.4226(4) 0.1555(3) 0.0360(12) Uani 1 1 d .
H6A H 0.4163 0.383 0.1661 0.043 Uiso 1 1 calc R
H6B H 0.2875 0.4154 0.2136 0.043 Uiso 1 1 calc R
C7 C 0.3594(4) 0.5466(4) 0.1333(3) 0.0286(11) Uani 1 1 d .
H7A H 0.4078 0.5822 0.1847 0.034 Uiso 1 1 calc R
H7B H 0.4063 0.5534 0.0737 0.034 Uiso 1 1 calc R
C8 C 0.0204(4) 0.7191(4) 0.0734(3) 0.0213(8) Uani 1 1 d .
H8A H -0.003(4) 0.768(4) 0.021(3) 0.026 Uiso 1 1 d .
H8B H 0.095(4) 0.758(3) 0.100(3) 0.026 Uiso 1 1 d .
C9 C -0.0750(3) 0.6499(3) 0.2217(3) 0.0186(9) Uani 1 1 d .
C10 C -0.2016(4) 0.7576(4) 0.1097(3) 0.0283(10) Uani 1 1 d .
H10A H -0.1958 0.7858 0.0438 0.034 Uiso 1 1 calc R
H10B H -0.2271 0.8222 0.1505 0.034 Uiso 1 1 calc R
C11 C -0.2957(4) 0.6627(4) 0.1153(3) 0.0337(11) Uani 1 1 d .
H11A H -0.3765 0.6915 0.0947 0.04 Uiso 1 1 calc R
H11B H -0.2719 0.5987 0.0732 0.04 Uiso 1 1 calc R
C12 C -0.3024(4) 0.6217(4) 0.2165(3) 0.0268(10) Uani 1 1 d .
H12A H -0.3551 0.6744 0.2533 0.032 Uiso 1 1 calc R
H12B H -0.3407 0.545 0.218 0.032 Uiso 1 1 calc R
C13 C -0.1860(4) 0.5590(4) 0.3544(3) 0.0262(9) Uani 1 1 d .
H13A H -0.2098 0.4779 0.3458 0.031 Uiso 1 1 calc R
H13B H -0.249 0.5964 0.394 0.031 Uiso 1 1 calc R
C14 C -0.0649(4) 0.5645(4) 0.4042(3) 0.0285(11) Uani 1 1 d .
H14A H -0.0624 0.5075 0.4561 0.034 Uiso 1 1 calc R
H14B H -0.0528 0.6415 0.432 0.034 Uiso 1 1 calc R
C15 C 0.0351(4) 0.5394(4) 0.3328(3) 0.0235(10) Uani 1 1 d .
H15A H 0.1157 0.5411 0.3646 0.028 Uiso 1 1 calc R
H15B H 0.0231 0.462 0.3058 0.028 Uiso 1 1 calc R
C16 C 0.1432(4) 0.8232(3) 0.3493(3) 0.0190(9) Uani 1 1 d .
H16A H 0.1072 0.8932 0.3231 0.028 Uiso 1 1 calc R
H16B H 0.2156 0.8428 0.3867 0.028 Uiso 1 1 calc R
H16C H 0.0832 0.7847 0.3898 0.028 Uiso 1 1 calc R
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 0 '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'
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
C16 Pd N5 90.44(14)
C16 Pd N1 178.61(15)
N5 Pd N1 89.39(13)
C16 Pd Cl 88.19(12)
N5 Pd Cl 173.45(9)
N1 Pd Cl 92.14(9)
C1 N1 C7 113.9(3)
C1 N1 Pd 125.8(3)
C7 N1 Pd 115.5(3)
C1 N2 C8 123.2(3)
C1 N2 C2 120.9(3)
C8 N2 C2 115.8(3)
C1 N3 C4 124.6(4)
C1 N3 C5 120.4(3)
C4 N3 C5 112.9(3)
C9 N4 C10 119.0(3)
C9 N4 C8 120.9(3)
C10 N4 C8 118.4(3)
C9 N5 C15 116.6(3)
C9 N5 Pd 127.0(2)
C15 N5 Pd 114.7(2)
C9 N6 C13 122.5(3)
C9 N6 C12 125.4(3)
C13 N6 C12 112.0(3)
N1 C1 N3 121.9(4)
N1 C1 N2 121.0(4)
N3 C1 N2 117.0(4)
N2 C2 C3 109.2(3)
C4 C3 C2 107.6(4)
N3 C4 C3 111.5(4)
N3 C5 C6 112.6(4)
C5 C6 C7 108.1(4)
N1 C7 C6 109.5(3)
N2 C8 N4 113.5(4)
N5 C9 N6 123.1(3)
N5 C9 N4 119.3(3)
N6 C9 N4 117.6(3)
N4 C10 C11 110.0(3)
C12 C11 C10 108.4(4)
N6 C12 C11 112.4(3)
N6 C13 C14 111.6(3)
C13 C14 C15 108.4(4)
N5 C15 C14 110.1(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd C16 2.057(4)
Pd N5 2.064(3)
Pd N1 2.161(3)
Pd Cl 2.3137(10)
N1 C1 1.315(5)
N1 C7 1.460(5)
N2 C1 1.382(5)
N2 C8 1.452(5)
N2 C2 1.463(5)
N3 C1 1.364(5)
N3 C4 1.462(5)
N3 C5 1.463(5)
N4 C9 1.376(5)
N4 C10 1.467(5)
N4 C8 1.470(5)
N5 C9 1.312(5)
N5 C15 1.462(5)
N6 C9 1.351(5)
N6 C13 1.469(5)
N6 C12 1.473(5)
C2 C3 1.507(6)
C3 C4 1.501(6)
C5 C6 1.492(6)
C6 C7 1.501(6)
C10 C11 1.514(6)
C11 C12 1.509(6)
C13 C14 1.501(6)
C14 C15 1.517(6)
