#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:48:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179765 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/61/7006112.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_7006112
loop_
_publ_author_name
'Clarke, Deborah A.'
'Miller, Philip W.'
'Long, Nicholas J.'
'White, Andrew J. P.'
_publ_section_title
;
 Steric control over the formation of cis and trans bis-chelated
 palladium(II) complexes using a new series of flexible N,P
 pyridyl-phosphine ligands.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4556
_journal_page_last               4564
_journal_paper_doi               10.1039/b709032c
_journal_year                    2007
_chemical_formula_moiety         'C38 H62 Cl2 N4 P2 Pd'
_chemical_formula_sum            'C38 H62 Cl2 N4 P2 Pd'
_chemical_formula_weight         814.16
_chemical_name_systematic
;
?
;
_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                 104.668(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.171(4)
_cell_length_b                   20.345(4)
_cell_length_c                   9.4447(8)
_cell_measurement_reflns_used    15930
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.9904
_cell_measurement_theta_min      3.8892
_cell_volume                     3935.5(11)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_data_collection
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 15.9863
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            28365
_diffrn_reflns_theta_full        32.06
_diffrn_reflns_theta_max         32.06
_diffrn_reflns_theta_min         3.90
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  1.01999
_exptl_absorpt_correction_T_min  0.98522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.204
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.067
_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     214
_refine_ls_number_reflns         6437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0293
_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)+(0.0460P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0756
_reflns_number_gt                4982
_reflns_number_total             6437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b709032c.txt
_cod_data_source_block           Compound_4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3935.4(11)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7006112
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_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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.0000 0.280666(7) 0.7500 0.01940(5) Uani 1 2 d S . .
Cl Cl 0.078793(17) 0.29031(2) 0.96771(4) 0.03081(9) Uani 1 1 d . . .
P P 0.081945(16) 0.274559(16) 0.62472(4) 0.01839(7) Uani 1 1 d . . .
C1 C 0.05660(8) 0.23045(7) 0.44610(16) 0.0255(3) Uani 1 1 d . . .
H1A H 0.0138 0.2481 0.3911 0.031 Uiso 1 1 calc R . .
H1B H 0.0886 0.2405 0.3888 0.031 Uiso 1 1 calc R . .
N2 N 0.05110(7) 0.15964(6) 0.45552(15) 0.0318(3) Uani 1 1 d . . .
C3 C 0.08551(7) 0.11861(7) 0.38686(16) 0.0286(3) Uani 1 1 d . . .
N4 N 0.12828(7) 0.14645(7) 0.32092(16) 0.0384(3) Uani 1 1 d . . .
C5 C 0.16072(9) 0.10670(11) 0.2505(2) 0.0501(5) Uani 1 1 d . . .
H5A H 0.1908 0.1260 0.2033 0.060 Uiso 1 1 calc R . .
C6 C 0.15281(10) 0.03939(11) 0.2427(2) 0.0599(6) Uani 1 1 d . . .
H6A H 0.1763 0.0130 0.1906 0.072 Uiso 1 1 calc R . .
C7 C 0.11017(10) 0.01206(10) 0.3124(3) 0.0594(6) Uani 1 1 d . . .
H7A H 0.1039 -0.0342 0.3095 0.071 Uiso 1 1 calc R . .
C8 C 0.07613(9) 0.05061(8) 0.3868(2) 0.0416(4) Uani 1 1 d . . .
H8A H 0.0470 0.0316 0.4369 0.050 Uiso 1 1 calc R . .
C9 C -0.00028(9) 0.13321(9) 0.5152(2) 0.0397(4) Uani 1 1 d . . .
H9A H -0.0298 0.1064 0.4408 0.060 Uiso 1 1 calc R . .
H9B H -0.0248 0.1694 0.5445 0.060 Uiso 1 1 calc R . .
H9C H 0.0190 0.1059 0.6008 0.060 Uiso 1 1 calc R . .
C10 C 0.15950(7) 0.23658(7) 0.72697(15) 0.0216(3) Uani 1 1 d . . .
H10A H 0.1762 0.2648 0.8152 0.026 Uiso 1 1 calc R . .
C11 C 0.15048(7) 0.16739(7) 0.78538(17) 0.0288(3) Uani 1 1 d . . .
H11A H 0.1176 0.1690 0.8435 0.035 Uiso 1 1 calc R . .
H11B H 0.1344 0.1370 0.7022 0.035 Uiso 1 1 calc R . .
C12 C 0.21526(8) 0.14211(8) 0.88103(19) 0.0360(4) Uani 1 1 d . . .
H12A H 0.2293 0.1706 0.9683 0.043 Uiso 1 1 calc R . .
H12B H 0.2091 0.0971 0.9150 0.043 Uiso 1 1 calc R . .
C13 C 0.26788(8) 0.14128(8) 0.7980(2) 0.0387(4) Uani 1 1 d . . .
H13A H 0.2556 0.1099 0.7156 0.046 Uiso 1 1 calc R . .
H13B H 0.3096 0.1264 0.8639 0.046 Uiso 1 1 calc R . .
C14 C 0.27681(7) 0.20950(8) 0.73945(18) 0.0310(3) Uani 1 1 d . . .
H14A H 0.3095 0.2073 0.6810 0.037 Uiso 1 1 calc R . .
H14B H 0.2936 0.2397 0.8226 0.037 Uiso 1 1 calc R . .
C15 C 0.21285(7) 0.23652(8) 0.64440(16) 0.0260(3) Uani 1 1 d . . .
H15A H 0.1987 0.2093 0.5551 0.031 Uiso 1 1 calc R . .
H15B H 0.2198 0.2819 0.6139 0.031 Uiso 1 1 calc R . .
C16 C 0.10651(7) 0.35509(6) 0.56734(14) 0.0215(3) Uani 1 1 d . . .
H16A H 0.1389 0.3468 0.5085 0.026 Uiso 1 1 calc R . .
C17 C 0.14033(8) 0.39757(7) 0.69819(16) 0.0285(3) Uani 1 1 d . . .
H17A H 0.1093 0.4075 0.7580 0.034 Uiso 1 1 calc R . .
H17B H 0.1776 0.3731 0.7602 0.034 Uiso 1 1 calc R . .
C18 C 0.16480(8) 0.46181(8) 0.64688(19) 0.0362(4) Uani 1 1 d . . .
H18A H 0.1846 0.4894 0.7330 0.043 Uiso 1 1 calc R . .
H18B H 0.1991 0.4519 0.5955 0.043 Uiso 1 1 calc R . .
C19 C 0.10971(9) 0.49957(8) 0.54478(19) 0.0368(4) Uani 1 1 d . . .
H19A H 0.0784 0.5147 0.5998 0.044 Uiso 1 1 calc R . .
H19B H 0.1277 0.5388 0.5070 0.044 Uiso 1 1 calc R . .
C20 C 0.07450(9) 0.45711(8) 0.41775(17) 0.0379(4) Uani 1 1 d . . .
H20A H 0.1046 0.4464 0.3561 0.046 Uiso 1 1 calc R . .
H20B H 0.0372 0.4819 0.3568 0.046 Uiso 1 1 calc R . .
C21 C 0.04957(8) 0.39345(8) 0.46998(17) 0.0305(3) Uani 1 1 d . . .
H21A H 0.0279 0.3663 0.3845 0.037 Uiso 1 1 calc R . .
H21B H 0.0170 0.4038 0.5258 0.037 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 0.0000 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'
P P 0.1023 0.0942 '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
_geom_angle_publ_flag
Cl Pd Cl 170.23(2) . 2_556 ?
Cl Pd P 90.870(18) . 2_556 ?
Cl Pd P 89.649(18) 2_556 2_556 ?
Cl Pd P 89.649(18) . . ?
Cl Pd P 90.870(18) 2_556 . ?
P Pd P 173.907(17) 2_556 . ?
C16 P C10 104.23(6) . . ?
C16 P C1 101.52(6) . . ?
C10 P C1 106.57(7) . . ?
C16 P Pd 113.75(4) . . ?
C10 P Pd 115.61(5) . . ?
C1 P Pd 113.76(5) . . ?
N2 C1 P 115.57(10) . . ?
C3 N2 C9 119.88(13) . . ?
C3 N2 C1 120.96(13) . . ?
C9 N2 C1 118.18(13) . . ?
N4 C3 N2 117.49(14) . . ?
N4 C3 C8 121.89(15) . . ?
N2 C3 C8 120.62(15) . . ?
C5 N4 C3 117.66(17) . . ?
N4 C5 C6 123.7(2) . . ?
C7 C6 C5 117.75(18) . . ?
C6 C7 C8 120.77(19) . . ?
C7 C8 C3 118.22(18) . . ?
C15 C10 C11 110.91(12) . . ?
C15 C10 P 114.04(10) . . ?
C11 C10 P 113.23(10) . . ?
C12 C11 C10 110.19(12) . . ?
C13 C12 C11 111.42(13) . . ?
C12 C13 C14 110.66(13) . . ?
C13 C14 C15 111.64(13) . . ?
C14 C15 C10 111.17(12) . . ?
C17 C16 C21 109.47(12) . . ?
C17 C16 P 111.98(9) . . ?
C21 C16 P 113.08(10) . . ?
C18 C17 C16 110.71(12) . . ?
C19 C18 C17 111.47(13) . . ?
C20 C19 C18 111.06(14) . . ?
C19 C20 C21 111.67(13) . . ?
C20 C21 C16 110.02(13) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd Cl 2.3048(5) . ?
Pd Cl 2.3048(5) 2_556 ?
Pd P 2.3376(5) 2_556 ?
Pd P 2.3376(5) . ?
P C16 1.8415(14) . ?
P C10 1.8500(14) . ?
P C1 1.8657(14) . ?
C1 N2 1.4499(18) . ?
N2 C3 1.3738(19) . ?
N2 C9 1.450(2) . ?
C3 N4 1.347(2) . ?
C3 C8 1.398(2) . ?
N4 C5 1.341(2) . ?
C5 C6 1.379(3) . ?
C6 C7 1.363(3) . ?
C7 C8 1.373(3) . ?
C10 C15 1.526(2) . ?
C10 C11 1.5412(19) . ?
C11 C12 1.528(2) . ?
C12 C13 1.516(2) . ?
C13 C14 1.524(2) . ?
C14 C15 1.525(2) . ?
C16 C17 1.5293(19) . ?
C16 C21 1.532(2) . ?
C17 C18 1.529(2) . ?
C18 C19 1.520(2) . ?
C19 C20 1.513(2) . ?
C20 C21 1.527(2) . ?
