#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:23:26 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179628 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/92/4509249.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_4509249
loop_
_publ_author_name
'Sluch, Ilya M.'
'Miranda, Anthea J.'
'Slaughter, LeGrande M.'
_publ_section_title
;
 Channeled Polymorphs ofcis-M(CNPh)2Cl2(M = Pt, Pd) With Extended
 Metallophilic Interactions
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1267
_journal_paper_doi               10.1021/cg801116q
_journal_volume                  9
_journal_year                    2009
_chemical_formula_moiety         'C14 H10 Cl2 N2 Pd'
_chemical_formula_sum            'C14 H10 Cl2 N2 Pd'
_chemical_formula_weight         383.54
_chemical_name_common            'Bis(phenylisocyanide) palladium dichloride'
_chemical_name_systematic        cis-Dichlorobis(phenylisocyanide)palladium(II)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 101.841(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9103(14)
_cell_length_b                   11.8010(17)
_cell_length_c                   12.7677(18)
_cell_measurement_reflns_used    7002
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      36.34
_cell_measurement_theta_min      2.38
_cell_volume                     1461.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL (XP)'
_computing_publication_material  'Bruker SHELXTL (XCIF)'
_computing_structure_refinement  'Bruker SHELXTL (XL)'
_computing_structure_solution    'Bruker SHELXTL (XS)'
_diffrn_ambient_temperature      115(2)
_diffrn_detector_area_resol_mean 0.75
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26004
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         2.10
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        N/A
_diffrn_standards_interval_count N/A
_diffrn_standards_interval_time  N/A
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.621
_exptl_absorpt_correction_T_max  0.7228
_exptl_absorpt_correction_T_min  0.5520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_recrystallization_method
'slow diff of n-hexane into dichloromethane soln'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         5578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0183
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0103P)²+0.5630P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0440
_refine_ls_wR_factor_ref         0.0454
_reflns_number_gt                5093
_reflns_number_total             5578
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg801116qsup1.cif
_cod_data_source_block           Complex_2b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4509249
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 0.454109(8) 0.469231(7) 0.617951(6) 0.01692(3) Uani 1 1 d .
C1 C 0.64001(12) 0.41913(11) 0.67863(10) 0.0231(2) Uani 1 1 d .
N1 N 0.74649(11) 0.38067(9) 0.71059(8) 0.0238(2) Uani 1 1 d .
C11 C 0.87444(12) 0.32715(10) 0.74568(9) 0.0211(2) Uani 1 1 d .
C12 C 0.88286(12) 0.24079(11) 0.82061(10) 0.0232(2) Uani 1 1 d .
H12 H 0.8047 0.2197 0.8486 0.028 Uiso 1 1 calc R
C13 C 1.00808(13) 0.18631(11) 0.85348(11) 0.0253(2) Uani 1 1 d .
H13 H 1.0166 0.1274 0.9052 0.030 Uiso 1 1 calc R
C14 C 1.12147(13) 0.21724(12) 0.81129(11) 0.0270(2) Uani 1 1 d .
H14 H 1.2068 0.1789 0.8338 0.032 Uiso 1 1 calc R
C15 C 1.11027(13) 0.30404(12) 0.73632(11) 0.0274(2) Uani 1 1 d .
H15 H 1.1882 0.3248 0.7080 0.033 Uiso 1 1 calc R
C16 C 0.98628(13) 0.36057(11) 0.70262(10) 0.0248(2) Uani 1 1 d .
H16 H 0.9779 0.4202 0.6517 0.030 Uiso 1 1 calc R
C2 C 0.40777(13) 0.31632(11) 0.56854(9) 0.0228(2) Uani 1 1 d .
N2 N 0.37477(12) 0.22665(9) 0.54013(8) 0.0248(2) Uani 1 1 d .
C21 C 0.32488(14) 0.11953(11) 0.50405(10) 0.0253(2) Uani 1 1 d .
C22 C 0.2273(2) 0.06969(14) 0.55269(12) 0.0395(4) Uani 1 1 d .
H22 H 0.1969 0.1064 0.6099 0.047 Uiso 1 1 calc R
C23 C 0.1752(2) -0.03493(15) 0.51605(14) 0.0504(5) Uani 1 1 d .
H23 H 0.1081 -0.0708 0.5482 0.060 Uiso 1 1 calc R
C24 C 0.2207(2) -0.08794(14) 0.43245(13) 0.0466(4) Uani 1 1 d .
H24 H 0.1849 -0.1601 0.4080 0.056 Uiso 1 1 calc R
C25 C 0.3176(2) -0.03627(13) 0.38479(12) 0.0394(4) Uani 1 1 d .
H25 H 0.3476 -0.0728 0.3273 0.047 Uiso 1 1 calc R
C26 C 0.37148(15) 0.06844(12) 0.42028(11) 0.0305(3) Uani 1 1 d .
H26 H 0.4386 0.1043 0.3881 0.037 Uiso 1 1 calc R
Cl1 Cl 0.50603(3) 0.65125(3) 0.68123(2) 0.02390(6) Uani 1 1 d .
Cl2 Cl 0.22871(3) 0.51509(3) 0.54375(2) 0.02376(6) Uani 1 1 d .
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_3
C2 Pd1 C1 89.34(5) .
C2 Pd1 Cl2 86.55(4) .
C1 Pd1 Cl2 175.82(4) .
C2 Pd1 Cl1 178.26(4) .
C1 Pd1 Cl1 91.06(4) .
Cl2 Pd1 Cl1 93.030(12) .
C2 Pd1 Pd1 89.95(4) 3_666
C1 Pd1 Pd1 90.81(4) 3_666
Cl2 Pd1 Pd1 89.922(12) 3_666
Cl1 Pd1 Pd1 91.735(10) 3_666
N1 C1 Pd1 174.11(12) .
C1 N1 C11 176.24(13) .
C12 C11 C16 122.69(11) .
C12 C11 N1 118.19(11) .
C16 C11 N1 119.10(11) .
C13 C12 C11 118.25(11) .
C13 C12 H12 120.9 .
C11 C12 H12 120.9 .
C12 C13 C14 120.40(12) .
C12 C13 H13 119.8 .
C14 C13 H13 119.8 .
C15 C14 C13 120.20(12) .
C15 C14 H14 119.9 .
C13 C14 H14 119.9 .
C16 C15 C14 120.55(12) .
C16 C15 H15 119.7 .
C14 C15 H15 119.7 .
C15 C16 C11 117.90(12) .
C15 C16 H16 121.1 .
C11 C16 H16 121.1 .
N2 C2 Pd1 177.04(11) .
C2 N2 C21 176.02(13) .
C22 C21 C26 122.37(13) .
C22 C21 N2 117.93(12) .
C26 C21 N2 119.68(12) .
C23 C22 C21 118.35(14) .
C23 C22 H22 120.8 .
C21 C22 H22 120.8 .
C22 C23 C24 120.32(16) .
C22 C23 H23 119.8 .
C24 C23 H23 119.8 .
C25 C24 C23 120.29(15) .
C25 C24 H24 119.9 .
C23 C24 H24 119.9 .
C24 C25 C26 120.41(14) .
C24 C25 H25 119.8 .
C26 C25 H25 119.8 .
C25 C26 C21 118.26(14) .
C25 C26 H26 120.9 .
C21 C26 H26 120.9 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C2 1.9355(13) .
Pd1 C1 1.9386(12) .
Pd1 Cl2 2.3047(4) .
Pd1 Cl1 2.3154(4) .
Pd1 Pd1 3.3986(4) 3_666
C1 N1 1.1443(16) .
N1 C11 1.4051(15) .
C11 C12 1.3884(17) .
C11 C16 1.3916(17) .
C12 C13 1.3841(17) .
C12 H12 0.9500 .
C13 C14 1.3909(19) .
C13 H13 0.9500 .
C14 C15 1.391(2) .
C14 H14 0.9500 .
C15 C16 1.3868(18) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C2 N2 1.1443(17) .
N2 C21 1.4004(17) .
C21 C22 1.383(2) .
C21 C26 1.3869(18) .
C22 C23 1.382(2) .
C22 H22 0.9500 .
C23 C24 1.390(2) .
C23 H23 0.9500 .
C24 C25 1.380(3) .
C24 H24 0.9500 .
C25 C26 1.385(2) .
C25 H25 0.9500 .
C26 H26 0.9500 .
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
C16 C11 C12 C13 0.11(19)
N1 C11 C12 C13 178.60(11)
C11 C12 C13 C14 -0.59(19)
C12 C13 C14 C15 0.6(2)
C13 C14 C15 C16 -0.1(2)
C14 C15 C16 C11 -0.4(2)
C12 C11 C16 C15 0.36(19)
N1 C11 C16 C15 -178.12(12)
C26 C21 C22 C23 0.1(3)
N2 C21 C22 C23 178.61(16)
C21 C22 C23 C24 0.1(3)
C22 C23 C24 C25 -0.4(3)
C23 C24 C25 C26 0.5(3)
C24 C25 C26 C21 -0.3(2)
C22 C21 C26 C25 0.0(2)
N2 C21 C26 C25 -178.46(13)
