#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:48:47 +0100 (vie 25 de mar de 2016) $
#$Revision: 179816 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/12/7011236.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_7011236
loop_
_publ_author_name
'Reddy, K. Rajender'
'Tsai, Wei-Wen'
'Surekha, K.'
'Lee, Gene-Hsiang'
'Peng, Shie-Ming'
'Chen, Jwu-Ting'
'Liu, Shiuh-Tzung'
_publ_section_title
;
 Ligand effects on palladium complex catalyzed copolymerization of
 ethylene/carbon monoxide
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1776
_journal_paper_doi               10.1039/b109290a
_journal_year                    2002
_chemical_formula_sum            'C26 H25 Cl N O P Pd'
_chemical_formula_weight         540.29
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.0520(10)
_cell_angle_beta                 101.3450(10)
_cell_angle_gamma                92.2640(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9142(2)
_cell_length_b                   10.3657(2)
_cell_length_c                   14.4963(3)
_cell_measurement_reflns_used    8960
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.48
_cell_volume                     1274.44(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_method       'ω scans'
_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  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16566
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.7261
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0503
_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)+(0.0532P)²+0.7492P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1233
_reflns_number_gt                4528
_reflns_number_total             5854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109290a.txt
_cod_data_source_block           ic5428
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

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_cell_volume        1274.43(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7011236
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.80527(4) 0.98873(3) 0.70750(2) 0.03229(11) Uani 1 1 d . . .
Cl Cl 0.97524(17) 1.16609(13) 0.81391(9) 0.0617(4) Uani 1 1 d . . .
P1 P 0.67083(12) 0.80819(10) 0.61351(8) 0.0321(2) Uani 1 1 d . . .
N1 N 0.7687(4) 0.9031(3) 0.8262(2) 0.0377(8) Uani 1 1 d . . .
C1 C 0.8320(6) 1.0691(4) 0.5950(3) 0.0458(11) Uani 1 1 d . . .
H1A H 0.7715 1.0148 0.5356 0.069 Uiso 1 1 calc R . .
H1B H 0.9382 1.0730 0.5911 0.069 Uiso 1 1 calc R . .
H1C H 0.7987 1.1572 0.6053 0.069 Uiso 1 1 calc R . .
C3 C 0.7693(4) 0.6715(4) 0.6528(3) 0.0361(9) Uani 1 1 d . . .
C4 C 0.8012(5) 0.5638(4) 0.5860(4) 0.0446(10) Uani 1 1 d . . .
H4A H 0.7710 0.5599 0.5202 0.054 Uiso 1 1 calc R . .
C5 C 0.8781(6) 0.4609(5) 0.6159(4) 0.0574(13) Uani 1 1 d . . .
H5A H 0.9005 0.3896 0.5704 0.069 Uiso 1 1 calc R . .
C6 C 0.9206(6) 0.4656(5) 0.7137(5) 0.0635(15) Uani 1 1 d . . .
H6A H 0.9728 0.3979 0.7344 0.076 Uiso 1 1 calc R . .
C7 C 0.8859(6) 0.5698(5) 0.7796(4) 0.0579(13) Uani 1 1 d . . .
H7A H 0.9108 0.5701 0.8451 0.069 Uiso 1 1 calc R . .
C8 C 0.8138(5) 0.6764(4) 0.7517(3) 0.0416(10) Uani 1 1 d . . .
C10 C 0.7822(5) 0.7820(5) 0.8298(3) 0.0456(11) Uani 1 1 d . . .
H10A H 0.7710 0.7590 0.8866 0.055 Uiso 1 1 calc R . .
C11 C 0.4793(4) 0.7872(4) 0.6361(3) 0.0327(8) Uani 1 1 d . . .
C12 C 0.4194(5) 0.6670(5) 0.6467(3) 0.0472(11) Uani 1 1 d . . .
H12A H 0.4782 0.5946 0.6427 0.057 Uiso 1 1 calc R . .
C13 C 0.2719(6) 0.6547(5) 0.6631(4) 0.0579(13) Uani 1 1 d . . .
H13A H 0.2322 0.5744 0.6709 0.070 Uiso 1 1 calc R . .
C14 C 0.1852(5) 0.7610(6) 0.6679(3) 0.0572(14) Uani 1 1 d . . .
H14A H 0.0858 0.7523 0.6780 0.069 Uiso 1 1 calc R . .
C15 C 0.2440(5) 0.8813(5) 0.6579(3) 0.0508(12) Uani 1 1 d . . .
H15A H 0.1848 0.9534 0.6617 0.061 Uiso 1 1 calc R . .
C16 C 0.3904(5) 0.8935(5) 0.6424(3) 0.0415(10) Uani 1 1 d . . .
H16A H 0.4301 0.9746 0.6361 0.050 Uiso 1 1 calc R . .
C21 C 0.6449(5) 0.7673(4) 0.4822(3) 0.0356(9) Uani 1 1 d . . .
C22 C 0.7732(5) 0.7781(5) 0.4413(3) 0.0457(11) Uani 1 1 d . . .
H22A H 0.8699 0.8044 0.4810 0.055 Uiso 1 1 calc R . .
C23 C 0.7558(6) 0.7495(5) 0.3417(4) 0.0556(13) Uani 1 1 d . . .
H23A H 0.8412 0.7549 0.3143 0.067 Uiso 1 1 calc R . .
C24 C 0.6120(7) 0.7131(6) 0.2830(4) 0.0629(15) Uani 1 1 d . . .
H24A H 0.6005 0.6953 0.2161 0.075 Uiso 1 1 calc R . .
C25 C 0.4869(7) 0.7029(6) 0.3223(4) 0.0632(14) Uani 1 1 d . . .
H25A H 0.3903 0.6779 0.2821 0.076 Uiso 1 1 calc R . .
C26 C 0.5023(5) 0.7295(5) 0.4220(3) 0.0456(11) Uani 1 1 d . . .
H26A H 0.4162 0.7219 0.4483 0.055 Uiso 1 1 calc R . .
C31 C 0.7336(6) 0.9918(5) 0.9086(3) 0.0458(11) Uani 1 1 d . . .
C32 C 0.6251(7) 1.0792(6) 0.8924(4) 0.0687(16) Uani 1 1 d . . .
H32A H 0.5796 1.0821 0.8295 0.082 Uiso 1 1 calc R . .
C33 C 0.5837(9) 1.1634(7) 0.9713(5) 0.087(2) Uani 1 1 d . . .
H33A H 0.5081 1.2210 0.9610 0.105 Uiso 1 1 calc R . .
C34 C 0.6545(9) 1.1615(8) 1.0638(5) 0.093(2) Uani 1 1 d . . .
H34A H 0.6270 1.2182 1.1162 0.112 Uiso 1 1 calc R . .
C35 C 0.7651(8) 1.0768(7) 1.0795(4) 0.0777(18) Uani 1 1 d . . .
H35A H 0.8144 1.0775 1.1424 0.093 Uiso 1 1 calc R . .
C36 C 0.8040(6) 0.9899(6) 1.0020(4) 0.0588(13) Uani 1 1 d . . .
H36A H 0.8771 0.9304 1.0128 0.071 Uiso 1 1 calc R . .
O1 O 0.8768(17) 0.3885(11) 0.9819(8) 0.140(5) Uani 0.510(12) 1 d P A 1
H1 H 0.7967 0.3792 0.9266 0.210 Uiso 0.51 1 d P A 1
H1' H 0.9400 0.4602 0.9979 0.210 Uiso 0.51 1 d P A 1
O2 O 0.7527(15) 0.6253(13) 1.0309(10) 0.146(5) Uani 0.490(12) 1 d P A 2
H2 H 0.7481 0.5641 1.0605 0.219 Uiso 0.49 1 d P A 2
H2' H 0.8148 0.5911 1.0057 0.219 Uiso 0.49 1 d P A 2
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'
O O 0.0106 0.0060 '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
C1 Pd N1 178.14(16) . . ?
C1 Pd P1 94.07(13) . . ?
N1 Pd P1 85.03(10) . . ?
C1 Pd Cl 88.71(13) . . ?
N1 Pd Cl 92.37(10) . . ?
P1 Pd Cl 172.74(5) . . ?
C11 P1 C21 105.00(19) . . ?
C11 P1 C3 104.33(19) . . ?
C21 P1 C3 105.35(19) . . ?
C11 P1 Pd 113.07(13) . . ?
C21 P1 Pd 123.07(14) . . ?
C3 P1 Pd 104.30(14) . . ?
C10 N1 C31 117.6(4) . . ?
C10 N1 Pd 125.5(3) . . ?
C31 N1 Pd 116.9(3) . . ?
C4 C3 C8 119.3(4) . . ?
C4 C3 P1 120.9(3) . . ?
C8 C3 P1 119.7(3) . . ?
C3 C4 C5 120.9(5) . . ?
C6 C5 C4 119.5(5) . . ?
C7 C6 C5 119.7(5) . . ?
C6 C7 C8 121.8(5) . . ?
C7 C8 C3 118.6(4) . . ?
C7 C8 C10 116.4(4) . . ?
C3 C8 C10 124.9(4) . . ?
N1 C10 C8 125.4(4) . . ?
C16 C11 C12 119.1(4) . . ?
C16 C11 P1 119.0(3) . . ?
C12 C11 P1 121.9(3) . . ?
C13 C12 C11 120.1(5) . . ?
C14 C13 C12 119.7(5) . . ?
C13 C14 C15 120.6(4) . . ?
C16 C15 C14 119.6(5) . . ?
C15 C16 C11 120.9(4) . . ?
C26 C21 C22 119.1(4) . . ?
C26 C21 P1 122.0(3) . . ?
C22 C21 P1 118.9(3) . . ?
C23 C22 C21 119.9(5) . . ?
C24 C23 C22 120.0(5) . . ?
C25 C24 C23 120.4(5) . . ?
C24 C25 C26 120.4(5) . . ?
C21 C26 C25 120.2(4) . . ?
C32 C31 C36 120.3(5) . . ?
C32 C31 N1 117.9(4) . . ?
C36 C31 N1 121.8(4) . . ?
C31 C32 C33 119.3(5) . . ?
C34 C33 C32 120.1(6) . . ?
C35 C34 C33 120.3(6) . . ?
C34 C35 C36 120.2(6) . . ?
C31 C36 C35 119.7(5) . . ?
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 C1 2.040(4) . ?
Pd N1 2.177(3) . ?
Pd P1 2.1963(11) . ?
Pd Cl 2.3737(12) . ?
P1 C11 1.815(4) . ?
P1 C21 1.820(4) . ?
P1 C3 1.835(4) . ?
N1 C10 1.277(5) . ?
N1 C31 1.430(6) . ?
C3 C4 1.382(6) . ?
C3 C8 1.399(6) . ?
C4 C5 1.395(6) . ?
C5 C6 1.383(8) . ?
C6 C7 1.361(7) . ?
C7 C8 1.397(6) . ?
C8 C10 1.466(6) . ?
C11 C16 1.380(6) . ?
C11 C12 1.388(6) . ?
C12 C13 1.388(7) . ?
C13 C14 1.368(8) . ?
C14 C15 1.381(7) . ?
C15 C16 1.373(6) . ?
C21 C26 1.379(6) . ?
C21 C22 1.399(6) . ?
C22 C23 1.383(7) . ?
C23 C24 1.377(8) . ?
C24 C25 1.359(8) . ?
C25 C26 1.386(6) . ?
C31 C32 1.374(7) . ?
C31 C36 1.381(7) . ?
C32 C33 1.395(8) . ?
C33 C34 1.371(9) . ?
C34 C35 1.366(9) . ?
C35 C36 1.383(8) . ?
