#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:48:47 +0100 (vie 25 de mar de 2016) $
#$Revision: 179816 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/12/7011237.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_7011237
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            'C19 H19 Cl N P Pd'
_chemical_formula_weight         434.17
_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                81.180(1)
_cell_angle_beta                 89.079(1)
_cell_angle_gamma                65.848(1)
_cell_formula_units_Z            2
_cell_length_a                   9.6838(3)
_cell_length_b                   9.8823(3)
_cell_length_c                   10.5044(3)
_cell_measurement_reflns_used    6151
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.96
_cell_volume                     905.19(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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9868
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    1.259
_exptl_absorpt_correction_T_max  0.8017
_exptl_absorpt_correction_T_min  0.6740
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.0025(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         4121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0246P)²+0.2566P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0621
_reflns_number_gt                3586
_reflns_number_total             4121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109290a.txt
_cod_data_source_block           ic5520
_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        905.20(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7011237
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 1.218506(18) 0.058192(19) 1.154995(17) 0.03299(7) Uani 1 1 d . . .
Cl Cl 1.26073(8) -0.11729(8) 1.01156(7) 0.05375(17) Uani 1 1 d . . .
N1 N 1.0183(2) 0.2209(2) 1.04063(18) 0.0384(4) Uani 1 1 d . . .
H1D H 1.0463 0.2454 0.9614 0.046 Uiso 1 1 calc R . .
H1E H 0.9546 0.1770 1.0317 0.046 Uiso 1 1 calc R . .
C1 C 1.4066(3) -0.0866(3) 1.2665(3) 0.0578(7) Uani 1 1 d . . .
H1A H 1.4144 -0.1873 1.2718 0.087 Uiso 1 1 calc R . .
H1B H 1.3990 -0.0605 1.3515 0.087 Uiso 1 1 calc R . .
H1C H 1.4950 -0.0801 1.2287 0.087 Uiso 1 1 calc R . .
P1 P 1.16798(6) 0.22723(7) 1.28151(6) 0.03229(13) Uani 1 1 d . . .
C3 C 0.9966(2) 0.3811(3) 1.2034(2) 0.0343(5) Uani 1 1 d . . .
C4 C 0.9201(3) 0.5149(3) 1.2521(3) 0.0464(6) Uani 1 1 d . . .
H4A H 0.9613 0.5329 1.3237 0.056 Uiso 1 1 calc R . .
C5 C 0.7841(3) 0.6203(3) 1.1946(3) 0.0521(7) Uani 1 1 d . . .
H5A H 0.7334 0.7088 1.2279 0.062 Uiso 1 1 calc R . .
C6 C 0.7228(3) 0.5951(3) 1.0876(3) 0.0515(7) Uani 1 1 d . . .
H6A H 0.6298 0.6656 1.0502 0.062 Uiso 1 1 calc R . .
C7 C 0.7991(3) 0.4656(3) 1.0360(2) 0.0438(6) Uani 1 1 d . . .
H7A H 0.7587 0.4499 0.9628 0.053 Uiso 1 1 calc R . .
C8 C 0.9364(2) 0.3586(3) 1.0936(2) 0.0341(5) Uani 1 1 d . . .
C11 C 1.1152(2) 0.1837(3) 1.4445(2) 0.0359(5) Uani 1 1 d . . .
C12 C 0.9672(3) 0.2046(3) 1.4697(3) 0.0473(6) Uani 1 1 d . . .
H12A H 0.8919 0.2479 1.4037 0.057 Uiso 1 1 calc R . .
C13 C 0.9320(3) 0.1611(3) 1.5930(3) 0.0599(8) Uani 1 1 d . . .
H13A H 0.8326 0.1760 1.6095 0.072 Uiso 1 1 calc R . .
C14 C 1.0417(4) 0.0965(3) 1.6907(3) 0.0575(7) Uani 1 1 d . . .
H14A H 1.0165 0.0688 1.7735 0.069 Uiso 1 1 calc R . .
C15 C 1.1876(4) 0.0727(3) 1.6669(3) 0.0593(8) Uani 1 1 d . . .
H15A H 1.2626 0.0267 1.7330 0.071 Uiso 1 1 calc R . .
C16 C 1.2248(3) 0.1170(3) 1.5443(2) 0.0508(6) Uani 1 1 d . . .
H16A H 1.3246 0.1017 1.5290 0.061 Uiso 1 1 calc R . .
C21 C 1.3048(2) 0.3062(3) 1.3005(2) 0.0350(5) Uani 1 1 d . . .
C22 C 1.2823(3) 0.4115(3) 1.3815(3) 0.0538(7) Uani 1 1 d . . .
H22A H 1.1998 0.4369 1.4336 0.065 Uiso 1 1 calc R . .
C23 C 1.3818(3) 0.4782(4) 1.3848(4) 0.0682(9) Uani 1 1 d . . .
H23A H 1.3662 0.5488 1.4390 0.082 Uiso 1 1 calc R . .
C24 C 1.5047(3) 0.4409(4) 1.3082(3) 0.0645(8) Uani 1 1 d . . .
H24A H 1.5702 0.4883 1.3091 0.077 Uiso 1 1 calc R . .
C25 C 1.5305(3) 0.3346(3) 1.2310(3) 0.0531(7) Uani 1 1 d . . .
H25A H 1.6150 0.3078 1.1812 0.064 Uiso 1 1 calc R . .
C26 C 1.4312(3) 0.2667(3) 1.2268(2) 0.0405(5) Uani 1 1 d . . .
H26A H 1.4495 0.1941 1.1742 0.049 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
C1 Pd N1 177.31(9) . . ?
C1 Pd P1 92.00(8) . . ?
N1 Pd P1 85.43(5) . . ?
C1 Pd Cl 91.03(8) . . ?
N1 Pd Cl 91.54(5) . . ?
P1 Pd Cl 176.94(2) . . ?
C8 N1 Pd 115.04(14) . . ?
C11 P1 C21 104.76(11) . . ?
C11 P1 C3 104.36(10) . . ?
C21 P1 C3 106.72(11) . . ?
C11 P1 Pd 118.05(8) . . ?
C21 P1 Pd 118.63(7) . . ?
C3 P1 Pd 102.91(8) . . ?
C8 C3 C4 119.1(2) . . ?
C8 C3 P1 117.30(17) . . ?
C4 C3 P1 123.53(19) . . ?
C5 C4 C3 120.3(3) . . ?
C4 C5 C6 120.2(2) . . ?
C7 C6 C5 120.2(2) . . ?
C6 C7 C8 119.9(2) . . ?
C3 C8 C7 120.2(2) . . ?
C3 C8 N1 119.11(19) . . ?
C7 C8 N1 120.7(2) . . ?
C16 C11 C12 118.5(2) . . ?
C16 C11 P1 120.24(18) . . ?
C12 C11 P1 121.01(19) . . ?
C13 C12 C11 119.9(3) . . ?
C14 C13 C12 120.7(3) . . ?
C15 C14 C13 120.0(3) . . ?
C14 C15 C16 120.1(3) . . ?
C11 C16 C15 120.7(3) . . ?
C26 C21 C22 118.9(2) . . ?
C26 C21 P1 119.08(18) . . ?
C22 C21 P1 121.97(18) . . ?
C23 C22 C21 120.2(2) . . ?
C22 C23 C24 120.3(3) . . ?
C25 C24 C23 120.1(3) . . ?
C24 C25 C26 120.2(2) . . ?
C25 C26 C21 120.3(2) . . ?
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 2.039(3) . ?
Pd N1 2.1724(19) . ?
Pd P1 2.1880(6) . ?
Pd Cl 2.3761(6) . ?
N1 C8 1.458(3) . ?
P1 C11 1.818(2) . ?
P1 C21 1.818(2) . ?
P1 C3 1.826(2) . ?
C3 C8 1.387(3) . ?
C3 C4 1.398(3) . ?
C4 C5 1.376(4) . ?
C5 C6 1.381(4) . ?
C6 C7 1.379(4) . ?
C7 C8 1.390(3) . ?
C11 C16 1.383(3) . ?
C11 C12 1.388(3) . ?
C12 C13 1.383(4) . ?
C13 C14 1.367(4) . ?
C14 C15 1.360(4) . ?
C15 C16 1.386(4) . ?
C21 C26 1.387(3) . ?
C21 C22 1.391(3) . ?
C22 C23 1.376(4) . ?
C23 C24 1.379(4) . ?
C24 C25 1.365(4) . ?
C25 C26 1.384(4) . ?
