#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:09:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179829 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/25/7012576.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_7012576
loop_
_publ_author_name
'Chen, Hsin-Pei'
'Liu, Yi-Hung'
'Peng, Shie-Ming'
'Liu, Shiuh-Tzung'
_publ_section_title
;
 New bulky phosphinopyridine ligands. P∼ N∼ C Tridentates in
 palladium complexes
;
_journal_issue                   7
_journal_name_full               'Dalton Transactions'
_journal_page_first              1419
_journal_paper_doi               10.1039/b212169g
_journal_year                    2003
_chemical_formula_sum            'C30 H38 B F4 N2 P Pd'
_chemical_formula_weight         650.80
_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                104.0900(10)
_cell_angle_beta                 94.3890(10)
_cell_angle_gamma                103.3000(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4710(2)
_cell_length_b                   12.1480(3)
_cell_length_c                   14.1510(4)
_cell_measurement_reflns_used    78403
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1521.56(7)
_computing_cell_refinement       'Denzo-SMN & Scalepack'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Denzo-SMN & Scalepack'
_computing_molecular_graphics    SHELX
_computing_publication_material  SHELX
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       'φ-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  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21100
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       0.0501(39)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.108
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         5323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_obs          0.0498
_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)+(0.0952P)²+0.5615P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1486
_refine_ls_wR_factor_obs         0.1355
_reflns_number_observed          4716
_reflns_number_total             5334
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b212169g.txt
_cod_data_source_block           ic8696
_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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+0.5615P] 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^)+(0.0952P)^2^+0.5615P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012576
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
Pd1 Pd -0.18608(3) 0.40987(2) 0.71008(2) 0.0494(2) Uani 1 d . .
P1 P 0.03476(11) 0.37235(9) 0.65469(8) 0.0469(3) Uani 1 d . .
N1 N -0.0500(3) 0.5518(3) 0.8033(2) 0.0462(7) Uani 1 d . .
N2 N -0.3521(4) 0.2748(4) 0.6316(3) 0.0637(9) Uani 1 d . .
C1 C -0.4569(5) 0.2046(4) 0.5962(4) 0.0645(11) Uani 1 d . .
C2 C -0.5929(6) 0.1174(5) 0.5532(4) 0.083(2) Uani 1 d . .
H2A H -0.5936(6) 0.0470(5) 0.5728(4) 0.125 Uiso 1 calc R .
H2B H -0.6019(6) 0.1004(5) 0.4828(4) 0.125 Uiso 1 calc R .
H2C H -0.6736(6) 0.1470(5) 0.5756(4) 0.125 Uiso 1 calc R .
C3 C 0.0959(4) 0.5876(3) 0.7974(3) 0.0466(8) Uani 1 d . .
C4 C 0.1863(4) 0.6817(3) 0.8673(3) 0.0511(9) Uani 1 d . .
H4A H 0.2856(4) 0.7036(3) 0.8622(3) 0.061 Uiso 1 calc R .
C5 C 0.1318(4) 0.7448(3) 0.9458(3) 0.0514(9) Uani 1 d . .
C6 C -0.0193(5) 0.7090(4) 0.9476(3) 0.0549(9) Uani 1 d . .
H6A H -0.0608(5) 0.7506(4) 0.9973(3) 0.066 Uiso 1 calc R .
C7 C -0.1068(4) 0.6143(3) 0.8779(3) 0.0517(9) Uani 1 d . .
C8 C -0.2687(4) 0.5643(4) 0.8789(3) 0.0573(10) Uani 1 d . .
C9 C -0.3370(5) 0.4868(4) 0.7753(4) 0.0620(11) Uani 1 d . .
H9A H -0.3689(5) 0.5342(4) 0.7361(4) 0.074 Uiso 1 calc R .
H9B H -0.4219(5) 0.4267(4) 0.7795(4) 0.074 Uiso 1 calc R .
C10 C -0.3479(6) 0.6633(5) 0.9080(4) 0.0788(15) Uani 1 d . .
H10A H -0.4500(6) 0.6293(5) 0.9080(4) 0.118 Uiso 1 calc R .
H10B H -0.3376(6) 0.7094(5) 0.8614(4) 0.118 Uiso 1 calc R .
H10C H -0.3052(6) 0.7125(5) 0.9725(4) 0.118 Uiso 1 calc R .
C11 C -0.2801(6) 0.4920(5) 0.9542(4) 0.0774(14) Uani 1 d . .
H11A H -0.3814(6) 0.4586(5) 0.9571(4) 0.116 Uiso 1 calc R .
H11B H -0.2338(6) 0.5419(5) 1.0178(4) 0.116 Uiso 1 calc R .
H11C H -0.2320(6) 0.4302(5) 0.9349(4) 0.116 Uiso 1 calc R .
C12 C 0.2276(5) 0.8506(4) 1.0245(3) 0.0614(11) Uani 1 d . .
C13 C 0.3894(6) 0.8514(5) 1.0303(5) 0.090(2) Uani 1 d . .
H13A H 0.4210(6) 0.8514(5) 0.9674(5) 0.135 Uiso 1 calc R .
H13B H 0.4029(6) 0.7829(5) 1.0483(5) 0.135 Uiso 1 calc R .
H13C H 0.4461(6) 0.9206(5) 1.0789(5) 0.135 Uiso 1 calc R .
C14 C 0.2131(8) 0.9601(5) 0.9955(7) 0.123(3) Uani 1 d . .
H14A H 0.2419(8) 0.9569(5) 0.9315(7) 0.185 Uiso 1 calc R .
H14B H 0.2751(8) 1.0282(5) 1.0426(7) 0.185 Uiso 1 calc R .
H14C H 0.1131(8) 0.9646(5) 0.9941(7) 0.185 Uiso 1 calc R .
C15 C 0.1837(11) 0.8508(8) 1.1248(5) 0.155(4) Uani 1 d . .
H15A H 0.1942(11) 0.7803(8) 1.1405(5) 0.232 Uiso 1 calc R .
H15B H 0.0834(11) 0.8543(8) 1.1246(5) 0.232 Uiso 1 calc R .
H15C H 0.2454(11) 0.9179(8) 1.1731(5) 0.232 Uiso 1 calc R .
C19 C 0.1493(4) 0.5246(3) 0.7078(3) 0.0519(9) Uani 1 d . .
H19A H 0.2495(4) 0.5225(3) 0.7253(3) 0.062 Uiso 1 calc R .
H19B H 0.1489(4) 0.5678(3) 0.6585(3) 0.062 Uiso 1 calc R .
C20 C 0.0576(5) 0.3336(3) 0.5250(3) 0.0522(9) Uani 1 d . .
C21 C -0.0702(5) 0.2834(4) 0.4591(3) 0.0603(11) Uani 1 d . .
H21A H -0.1598(5) 0.2794(4) 0.4827(3) 0.072 Uiso 1 calc R .
C22 C -0.0693(6) 0.2384(4) 0.3586(3) 0.0697(13) Uani 1 d . .
H22A H -0.1563(6) 0.2038(4) 0.3156(3) 0.084 Uiso 1 calc R .
C23 C 0.0641(7) 0.2468(4) 0.3252(4) 0.0758(14) Uani 1 d . .
H23A H 0.0673(7) 0.2162(4) 0.2587(4) 0.091 Uiso 1 calc R .
C24 C 0.1939(7) 0.3000(5) 0.3887(4) 0.0723(13) Uani 1 d . .
H24A H 0.2823(7) 0.3055(5) 0.3634(4) 0.087 Uiso 1 calc R .
C25 C 0.1960(5) 0.3453(4) 0.4890(3) 0.0593(10) Uani 1 d . .
C26 C 0.3395(5) 0.4054(5) 0.5522(4) 0.0747(13) Uani 1 d . .
H26A H 0.3236(5) 0.4319(5) 0.6192(4) 0.112 Uiso 1 calc R .
H26B H 0.3871(5) 0.4715(5) 0.5303(4) 0.112 Uiso 1 calc R .
H26C H 0.4001(5) 0.3515(5) 0.5478(4) 0.112 Uiso 1 calc R .
C30 C 0.1205(4) 0.2766(3) 0.7074(3) 0.0485(8) Uani 1 d . .
C31 C 0.2501(5) 0.3216(4) 0.7750(3) 0.0599(10) Uani 1 d . .
H31A H 0.2922(5) 0.4022(4) 0.7947(3) 0.072 Uiso 1 calc R .
C32 C 0.3160(5) 0.2476(5) 0.8128(4) 0.0739(13) Uani 1 d . .
H32A H 0.4022(5) 0.2786(5) 0.8569(4) 0.089 Uiso 1 calc R .
C33 C 0.2541(7) 0.1288(5) 0.7851(4) 0.0796(15) Uani 1 d . .
H33A H 0.3002(7) 0.0788(5) 0.8084(4) 0.096 Uiso 1 calc R .
C34 C 0.1262(6) 0.0846(4) 0.7239(4) 0.0740(13) Uani 1 d . .
H34A H 0.0830(6) 0.0044(4) 0.7092(4) 0.089 Uiso 1 calc R .
C35 C 0.0549(5) 0.1543(4) 0.6811(3) 0.0553(9) Uani 1 d . .
C36 C -0.0871(6) 0.0979(4) 0.6136(4) 0.0761(14) Uani 1 d . .
H36A H -0.1213(6) 0.1567(4) 0.5908(4) 0.114 Uiso 1 calc R .
H36B H -0.1586(6) 0.0611(4) 0.6485(4) 0.114 Uiso 1 calc R .
H36C H -0.0723(6) 0.0399(4) 0.5584(4) 0.114 Uiso 1 calc R .
B1 B 0.4877(7) 0.8418(6) 0.7037(5) 0.076(2) Uani 1 d . .
F1 F 0.4403(13) 0.8914(11) 0.6417(9) 0.307(6) Uani 1 d . .
F2 F 0.4176(7) 0.8771(6) 0.7771(4) 0.177(3) Uani 1 d . .
F3 F 0.6297(6) 0.8811(6) 0.7167(6) 0.216(4) Uani 1 d . .
F4 F 0.4402(7) 0.7364(6) 0.6546(7) 0.234(4) Uani 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'
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'
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'
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
N1 Pd1 N2 169.22(13) . . ?
N1 Pd1 C9 80.9(2) . . ?
N2 Pd1 C9 88.6(2) . . ?
N1 Pd1 P1 83.71(9) . . ?
N2 Pd1 P1 106.89(11) . . ?
C9 Pd1 P1 164.12(13) . . ?
C20 P1 C30 104.5(2) . . ?
C20 P1 C19 106.1(2) . . ?
C30 P1 C19 107.1(2) . . ?
C20 P1 Pd1 122.91(14) . . ?
C30 P1 Pd1 118.45(13) . . ?
C19 P1 Pd1 95.71(12) . . ?
C3 N1 C7 118.9(3) . . ?
C3 N1 Pd1 123.6(3) . . ?
C7 N1 Pd1 117.5(3) . . ?
C1 N2 Pd1 170.8(4) . . ?
N2 C1 C2 178.1(5) . . ?
N1 C3 C4 121.1(4) . . ?
N1 C3 C19 116.7(3) . . ?
C4 C3 C19 122.1(3) . . ?
C3 C4 C5 121.1(4) . . ?
C4 C5 C6 116.5(4) . . ?
C4 C5 C12 123.0(4) . . ?
C6 C5 C12 120.5(4) . . ?
C7 C6 C5 121.3(4) . . ?
N1 C7 C6 121.0(4) . . ?
N1 C7 C8 114.2(4) . . ?
C6 C7 C8 124.7(4) . . ?
C7 C8 C11 106.8(4) . . ?
C7 C8 C9 108.4(4) . . ?
C11 C8 C9 111.1(4) . . ?
C7 C8 C10 111.2(4) . . ?
C11 C8 C10 110.2(4) . . ?
C9 C8 C10 109.0(4) . . ?
C8 C9 Pd1 109.6(3) . . ?
C15 C12 C14 111.9(7) . . ?
C15 C12 C5 110.9(4) . . ?
C14 C12 C5 107.6(4) . . ?
C15 C12 C13 107.3(6) . . ?
C14 C12 C13 107.0(5) . . ?
C5 C12 C13 112.1(4) . . ?
C3 C19 P1 112.4(3) . . ?
C21 C20 C25 119.3(4) . . ?
C21 C20 P1 115.9(3) . . ?
C25 C20 P1 124.7(3) . . ?
C20 C21 C22 122.3(5) . . ?
C23 C22 C21 117.9(5) . . ?
C22 C23 C24 121.3(5) . . ?
C23 C24 C25 122.0(5) . . ?
C24 C25 C20 117.2(5) . . ?
C24 C25 C26 119.0(4) . . ?
C20 C25 C26 123.8(4) . . ?
C31 C30 C35 118.8(4) . . ?
C31 C30 P1 121.5(3) . . ?
C35 C30 P1 119.7(3) . . ?
C32 C31 C30 120.9(4) . . ?
C33 C32 C31 120.1(5) . . ?
C34 C33 C32 119.8(5) . . ?
C33 C34 C35 123.1(5) . . ?
C34 C35 C30 117.2(4) . . ?
C34 C35 C36 119.7(4) . . ?
C30 C35 C36 123.1(4) . . ?
F4 B1 F1 99.1(9) . . ?
F4 B1 F3 114.7(6) . . ?
F1 B1 F3 105.3(8) . . ?
F4 B1 F2 116.1(7) . . ?
F1 B1 F2 99.8(7) . . ?
F3 B1 F2 117.7(6) . . ?
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
Pd1 N1 1.996(3) . ?
Pd1 N2 2.014(4) . ?
Pd1 C9 2.041(4) . ?
Pd1 P1 2.3900(10) . ?
P1 C20 1.822(4) . ?
P1 C30 1.826(4) . ?
P1 C19 1.854(4) . ?
N1 C3 1.366(5) . ?
N1 C7 1.366(5) . ?
N2 C1 1.136(6) . ?
C1 C2 1.445(7) . ?
C3 C4 1.373(6) . ?
C3 C19 1.500(5) . ?
C4 C5 1.394(6) . ?
C5 C6 1.401(6) . ?
C5 C12 1.526(6) . ?
C6 C7 1.367(6) . ?
C7 C8 1.517(5) . ?
C8 C11 1.533(7) . ?
C8 C9 1.535(6) . ?
C8 C10 1.549(6) . ?
C12 C15 1.509(8) . ?
C12 C14 1.515(7) . ?
C12 C13 1.526(7) . ?
C20 C21 1.385(6) . ?
C20 C25 1.432(6) . ?
C21 C22 1.395(7) . ?
C22 C23 1.373(8) . ?
C23 C24 1.385(8) . ?
C24 C25 1.389(7) . ?
C25 C26 1.490(7) . ?
C30 C31 1.406(6) . ?
C30 C35 1.415(6) . ?
C31 C32 1.387(6) . ?
C32 C33 1.372(8) . ?
C33 C34 1.349(8) . ?
C34 C35 1.410(6) . ?
C35 C36 1.500(6) . ?
B1 F4 1.256(8) . ?
B1 F1 1.287(10) . ?
B1 F3 1.302(8) . ?
B1 F2 1.313(8) . ?
