#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/74/4077424.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_4077424
loop_
_publ_author_name
'Reddy, K. Rajender'
'Surekha, K.'
'Lee, Gene-Hsiang'
'Peng, Shie-Ming'
'Liu, Shiuh-Tzung'
_publ_section_title
;
 Single and Multiple Insertion of Alkynes into Pd−Acyl and
 Pd−Aryl Bonds in Cationic Palladium Complexes with
 Phosphine−Imine (P∼ N) Ligands
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              5557
_journal_paper_doi               10.1021/om0106377
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C31.5 H28 B Cl F4 N O3 P Pd'
_chemical_formula_weight         728.18
_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
_cell_angle_alpha                114.151(1)
_cell_angle_beta                 116.522(1)
_cell_angle_gamma                94.510(1)
_cell_formula_units_Z            2
_cell_length_a                   12.5765(1)
_cell_length_b                   12.7653(2)
_cell_length_c                   12.7816(1)
_cell_measurement_reflns_used    7475
_cell_measurement_temperature    295(2)
_cell_volume                     1587.20(4)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_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    0.0279
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19497
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.8017
_exptl_absorpt_correction_T_min  0.6869
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             734
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.0001(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.026
_refine_ls_goodness_of_fit_obs   1.047
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_restrained_S_obs      1.047
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_obs          0.0389
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0625P)²+1.5601P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1132
_refine_ls_wR_factor_obs         0.1081
_reflns_number_observed          5713
_reflns_number_total             6486
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om0106377.cif
_cod_data_source_block           ic5967
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+1.5601P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+1.5601P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1587.20(3)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C31.50 H28 B Cl F4 N O3 P Pd'
_cod_database_code               4077424
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pd Pd 0.82001(2) 0.94867(2) 0.70936(2) 0.04066(10) Uani 1 d . .
P1 P 0.83895(8) 0.77116(7) 0.68809(8) 0.0416(2) Uani 1 d . .
O1 O 0.8107(2) 1.1266(2) 0.7494(3) 0.0543(6) Uani 1 d . .
O2 O 0.5187(3) 0.7288(3) 0.5626(3) 0.0822(9) Uani 1 d . .
O3 O 0.5502(3) 0.8495(3) 0.7656(3) 0.0763(9) Uani 1 d . .
N1 N 0.9988(2) 0.9750(2) 0.7308(3) 0.0444(6) Uani 1 d . .
C1 C 0.6722(5) 1.2416(4) 0.7298(6) 0.0806(13) Uani 1 d . .
H1A H 0.7421(5) 1.2987(4) 0.7493(6) 0.121 Uiso 1 calc R .
H1B H 0.6522(5) 1.2777(4) 0.7980(6) 0.121 Uiso 1 calc R .
H1C H 0.6010(5) 1.2193(4) 0.6435(6) 0.121 Uiso 1 calc R .
C2 C 0.7051(4) 1.1322(3) 0.7277(4) 0.0538(8) Uani 1 d . .
C3 C 0.6177(4) 1.0301(3) 0.7009(4) 0.0568(9) Uani 1 d . .
H3A H 0.5398(4) 1.0322(3) 0.6898(4) 0.068 Uiso 1 calc R .
C4 C 0.6538(3) 0.9322(3) 0.6925(3) 0.0471(7) Uani 1 d . .
C5 C 0.5662(3) 0.8254(3) 0.6642(4) 0.0522(8) Uani 1 d . .
C6 C 0.4667(5) 0.7534(5) 0.7525(7) 0.097(2) Uani 1 d . .
H6A H 0.4632(5) 0.7824(5) 0.8327(7) 0.146 Uiso 1 calc R .
H6B H 0.4975(5) 0.6855(5) 0.7401(7) 0.146 Uiso 1 calc R .
H6C H 0.3842(5) 0.7288(5) 0.6761(7) 0.146 Uiso 1 calc R .
C7 C 1.0451(3) 1.0399(3) 0.6972(3) 0.0490(8) Uani 1 d . .
H7A H 1.1288(3) 1.0513(3) 0.7228(3) 0.059 Uiso 1 calc R .
C8 C 0.9769(3) 1.0972(3) 0.6220(3) 0.0490(7) Uani 1 d . .
C9 C 0.8493(3) 1.0462(3) 0.5244(4) 0.0544(8) Uani 1 d . .
H9A H 0.8038(3) 0.9729(3) 0.5050(4) 0.065 Uiso 1 calc R .
C10 C 0.7908(4) 1.1047(4) 0.4566(5) 0.0705(11) Uani 1 d . .
H10A H 0.7054(4) 1.0711(4) 0.3918(5) 0.085 Uiso 1 calc R .
C11 C 0.8584(5) 1.2129(5) 0.4843(6) 0.0863(15) Uani 1 d . .
H11A H 0.8182(5) 1.2533(5) 0.4401(6) 0.104 Uiso 1 calc R .
C12 C 0.9852(5) 1.2611(5) 0.5775(6) 0.089(2) Uani 1 d . .
H12A H 1.0309(5) 1.3331(5) 0.5943(6) 0.107 Uiso 1 calc R .
C13 C 1.0448(4) 1.2041(4) 0.6456(5) 0.0674(11) Uani 1 d . .
H13A H 1.1307(4) 1.2368(4) 0.7078(5) 0.081 Uiso 1 calc R .
C14 C 1.0746(3) 0.9171(3) 0.7978(3) 0.0455(7) Uani 1 d . .
C15 C 1.2056(3) 0.9583(4) 0.8726(4) 0.0586(9) Uani 1 d . .
H15A H 1.2498(3) 1.0262(4) 0.8811(4) 0.070 Uiso 1 calc R .
C16 C 1.2682(4) 0.8968(4) 0.9334(4) 0.0689(11) Uani 1 d . .
H16A H 1.3555(4) 0.9232(4) 0.9820(4) 0.083 Uiso 1 calc R .
C17 C 1.2048(4) 0.7970(4) 0.9240(4) 0.0689(11) Uani 1 d . .
H17A H 1.2493(4) 0.7571(4) 0.9664(4) 0.083 Uiso 1 calc R .
C18 C 1.0757(4) 0.7565(4) 0.8518(4) 0.0597(9) Uani 1 d . .
H18A H 1.0329(4) 0.6893(4) 0.8456(4) 0.072 Uiso 1 calc R .
C19 C 1.0089(3) 0.8162(3) 0.7880(3) 0.0463(7) Uani 1 d . .
C20 C 0.7816(3) 0.6985(3) 0.7569(3) 0.0489(7) Uani 1 d . .
C21 C 0.8233(5) 0.7604(4) 0.8930(4) 0.0742(13) Uani 1 d . .
H21A H 0.8813(5) 0.8379(4) 0.9485(4) 0.089 Uiso 1 calc R .
C22 C 0.7788(6) 0.7069(5) 0.9459(5) 0.092(2) Uani 1 d . .
H22A H 0.8079(6) 0.7486(5) 1.0375(5) 0.110 Uiso 1 calc R .
C23 C 0.6926(5) 0.5939(4) 0.8663(5) 0.0779(13) Uani 1 d . .
H23A H 0.6626(5) 0.5593(4) 0.9034(5) 0.093 Uiso 1 calc R .
C24 C 0.6503(4) 0.5317(4) 0.7318(5) 0.0642(10) Uani 1 d . .
H24A H 0.5924(4) 0.4542(4) 0.6774(5) 0.077 Uiso 1 calc R .
C25 C 0.6937(4) 0.5839(3) 0.6760(4) 0.0537(8) Uani 1 d . .
H25A H 0.6637(4) 0.5418(3) 0.5842(4) 0.064 Uiso 1 calc R .
C26 C 0.7902(3) 0.6544(3) 0.5194(3) 0.0435(7) Uani 1 d . .
C27 C 0.8414(4) 0.5596(3) 0.5005(4) 0.0520(8) Uani 1 d . .
H27A H 0.9006(4) 0.5559(3) 0.5745(4) 0.062 Uiso 1 calc R .
C28 C 0.8036(4) 0.4718(3) 0.3714(4) 0.0596(9) Uani 1 d . .
H28A H 0.8378(4) 0.4089(3) 0.3588(4) 0.071 Uiso 1 calc R .
C29 C 0.7171(4) 0.4763(4) 0.2629(4) 0.0657(11) Uani 1 d . .
H29A H 0.6919(4) 0.4161(4) 0.1765(4) 0.079 Uiso 1 calc R .
C30 C 0.6663(4) 0.5695(4) 0.2796(4) 0.0679(11) Uani 1 d . .
H30A H 0.6074(4) 0.5723(4) 0.2047(4) 0.081 Uiso 1 calc R .
C31 C 0.7032(3) 0.6593(3) 0.4086(3) 0.0540(8) Uani 1 d . .
H31A H 0.6694(3) 0.7225(3) 0.4202(3) 0.065 Uiso 1 calc R .
B1 B 0.5659(4) 0.7870(5) 0.1427(5) 0.0663(12) Uani 1 d . .
F1 F 0.5981(3) 0.8295(3) 0.2759(3) 0.1018(9) Uani 1 d . .
F2 F 0.5451(5) 0.8798(5) 0.1154(5) 0.159(2) Uani 1 d . .
F3 F 0.4594(4) 0.6979(5) 0.0673(4) 0.159(2) Uani 1 d . .
F4 F 0.6620(4) 0.7618(5) 0.1355(5) 0.148(2) Uani 1 d . .
C32 C 1.0053(6) 0.4924(6) 0.9259(6) 0.220(2) Uiso 0.50 d P 1
H32A H 0.9460 0.4265 0.8525 0.264 Uiso 0.50 d P 1
H32B H 0.9849 0.5645 0.9229 0.264 Uiso 0.50 d P 1
Cl2 Cl 1.0053(6) 0.4924(6) 0.9259(6) 0.220(2) Uiso 0.50 d P 1
Cl1 Cl 1.1078(7) 0.5041(7) 0.9130(7) 0.202(2) Uiso 0.50 d P .
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'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
C4 Pd N1 177.33(12) . .
C4 Pd O1 79.99(12) . .
N1 Pd O1 97.38(10) . .
C4 Pd P1 100.28(10) . .
N1 Pd P1 82.30(8) . .
O1 Pd P1 174.76(7) . .
C20 P1 C26 106.56(15) . .
C20 P1 C19 106.1(2) . .
C26 P1 C19 106.7(2) . .
C20 P1 Pd 121.73(11) . .
C26 P1 Pd 115.44(11) . .
C19 P1 Pd 98.58(11) . .
C2 O1 Pd 110.8(2) . .
C5 O3 C6 117.7(4) . .
C7 N1 C14 119.4(3) . .
C7 N1 Pd 126.9(2) . .
C14 N1 Pd 113.6(2) . .
O1 C2 C3 118.3(3) . .
O1 C2 C1 119.7(4) . .
C3 C2 C1 122.0(3) . .
C4 C3 C2 117.3(3) . .
C3 C4 C5 118.7(3) . .
C3 C4 Pd 112.8(3) . .
C5 C4 Pd 128.3(2) . .
O2 C5 O3 124.7(4) . .
O2 C5 C4 123.9(4) . .
O3 C5 C4 111.3(3) . .
N1 C7 C8 125.2(3) . .
C13 C8 C9 119.4(3) . .
C13 C8 C7 117.8(3) . .
C9 C8 C7 122.7(3) . .
C10 C9 C8 119.7(4) . .
C9 C10 C11 120.2(4) . .
C12 C11 C10 120.0(4) . .
C13 C12 C11 120.5(4) . .
C12 C13 C8 120.0(4) . .
C15 C14 C19 120.1(3) . .
C15 C14 N1 123.9(3) . .
C19 C14 N1 116.0(3) . .
C16 C15 C14 118.9(4) . .
C15 C16 C17 121.6(4) . .
C18 C17 C16 119.9(4) . .
C17 C18 C19 120.1(4) . .
C18 C19 C14 119.4(3) . .
C18 C19 P1 124.5(3) . .
C14 C19 P1 116.1(2) . .
C25 C20 C21 118.9(3) . .
C25 C20 P1 121.7(3) . .
C21 C20 P1 119.4(3) . .
C22 C21 C20 119.9(4) . .
C23 C22 C21 121.2(4) . .
C22 C23 C24 119.6(4) . .
C23 C24 C25 120.2(4) . .
C20 C25 C24 120.1(3) . .
C31 C26 C27 119.5(3) . .
C31 C26 P1 120.1(3) . .
C27 C26 P1 120.4(3) . .
C28 C27 C26 119.6(3) . .
C29 C28 C27 120.6(4) . .
C28 C29 C30 120.5(4) . .
C29 C30 C31 119.9(4) . .
C26 C31 C30 119.8(4) . .
F4 B1 F3 117.6(6) . .
F4 B1 F2 109.7(5) . .
F3 B1 F2 108.5(4) . .
F4 B1 F1 107.3(4) . .
F3 B1 F1 106.1(4) . .
F2 B1 F1 107.2(5) . .
Cl1 C32 Cl2 130.2(7) . 2_767
Cl1 C32 C32 130.2(7) . 2_767
Cl2 C32 C32 0.0(7) 2_767 2_767
Cl1 Cl2 Cl2 130.2(7) . 2_767
Cl1 Cl2 C32 130.2(7) . 2_767
Cl2 Cl2 C32 0.0(7) 2_767 2_767
Cl2 Cl1 C32 0.0(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd C4 1.988(3) .
Pd N1 2.121(3) .
Pd O1 2.140(2) .
Pd P1 2.2145(8) .
P1 C20 1.812(3) .
P1 C26 1.814(3) .
P1 C19 1.816(3) .
O1 C2 1.244(4) .
O2 C5 1.202(5) .
O3 C5 1.316(5) .
O3 C6 1.452(5) .
N1 C7 1.284(4) .
N1 C14 1.445(4) .
C1 C2 1.480(5) .
C2 C3 1.447(5) .
C3 C4 1.343(5) .
C4 C5 1.486(5) .
C7 C8 1.461(5) .
C8 C13 1.390(5) .
C8 C9 1.392(5) .
C9 C10 1.378(6) .
C10 C11 1.378(7) .
C11 C12 1.375(7) .
C12 C13 1.368(7) .
C14 C15 1.397(5) .
C14 C19 1.402(5) .
C15 C16 1.374(6) .
C16 C17 1.380(7) .
C17 C18 1.377(6) .
C18 C19 1.396(5) .
C20 C25 1.385(5) .
C20 C21 1.386(5) .
C21 C22 1.374(6) .
C22 C23 1.364(7) .
C23 C24 1.368(7) .
C24 C25 1.387(5) .
C26 C31 1.381(5) .
C26 C27 1.400(5) .
C27 C28 1.381(5) .
C28 C29 1.356(6) .
C29 C30 1.380(6) .
C30 C31 1.390(5) .
B1 F4 1.307(6) .
B1 F3 1.315(6) .
B1 F2 1.379(7) .
B1 F1 1.397(6) .
C32 Cl1 1.375(8) .
C32 Cl2 1.889(12) 2_767
C32 C32 1.889(12) 2_767
Cl2 Cl1 1.375(8) .
Cl2 Cl2 1.889(12) 2_767
Cl2 C32 1.889(12) 2_767
