#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:19:14 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179017 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/15/4121534.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_4121534
loop_
_publ_author_name
'Xue, Ya-Xin'
'Zhu, Yuan-Yuan'
'Gao, Long-Mei'
'He, Xiao-Yue'
'Liu, Na'
'Zhang, Wu-Yi'
'Yin, Jun'
'Ding, Yunsheng'
'Zhou, Hongping'
'Wu, Zong-Quan'
_publ_section_title
;
 Air-Stable (Phenylbuta-1,3-diynyl)palladium(II) Complexes: Highly Active
 Initiators for Living Polymerization of Isocyanides.
;
_journal_issue                   12
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4706
_journal_page_last               4713
_journal_paper_doi               10.1021/ja5004747
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         C23H37ClP2Pd
_chemical_formula_sum            'C23 H37 Cl P2 Pd'
_chemical_formula_weight         517.32
_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                93.4450(10)
_cell_angle_beta                 90.9690(10)
_cell_angle_gamma                101.9840(10)
_cell_formula_units_Z            2
_cell_length_a                   8.4589(10)
_cell_length_b                   10.5591(12)
_cell_length_c                   14.9611(18)
_cell_measurement_reflns_used    7595
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.08
_cell_measurement_theta_min      2.33
_cell_volume                     1304.2(3)
_computing_cell_refinement       'Bruker SMART'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9920
_diffrn_reflns_theta_full        26.08
_diffrn_reflns_theta_max         26.08
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    0.942
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         5003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0229
_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)+(0.0309P)²+0.4723P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0698
_reflns_number_gt                4617
_reflns_number_total             5003
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5004747_si_002.cif
_cod_data_source_block           1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4121534
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
Pd Pd 0.008053(17) 0.120054(15) 0.257023(10) 0.03869(7) Uani 1 1 d .
P2 P 0.17085(7) -0.01824(6) 0.29944(4) 0.04471(13) Uani 1 1 d .
P1 P -0.14929(7) 0.25915(6) 0.20717(4) 0.04593(14) Uani 1 1 d .
Cl1 Cl -0.18494(8) 0.05667(7) 0.36492(4) 0.06399(17) Uani 1 1 d .
C1 C 0.1593(3) 0.1694(2) 0.16191(15) 0.0453(5) Uani 1 1 d .
C5 C 0.4371(3) 0.3162(2) -0.13204(15) 0.0478(5) Uani 1 1 d .
C9 C 0.5909(3) 0.4795(3) -0.22030(18) 0.0589(6) Uani 1 1 d .
H9 H 0.6657 0.5573 -0.2229 0.071 Uiso 1 1 calc R
C20 C 0.0850(3) -0.1324(3) 0.38168(18) 0.0598(6) Uani 1 1 d .
H20A H 0.0596 -0.0833 0.4344 0.072 Uiso 1 1 calc R
H20B H -0.0158 -0.1848 0.3568 0.072 Uiso 1 1 calc R
C14 C -0.0626(3) 0.3756(3) 0.1272(2) 0.0631(7) Uani 1 1 d .
H14A H 0.0301 0.4346 0.1558 0.076 Uiso 1 1 calc R
H14B H -0.0234 0.3289 0.0773 0.076 Uiso 1 1 calc R
C10 C 0.5485(3) 0.4323(2) -0.13811(16) 0.0541(6) Uani 1 1 d .
H10 H 0.5950 0.4787 -0.0861 0.065 Uiso 1 1 calc R
C3 C 0.3176(3) 0.2380(2) 0.02092(15) 0.0503(5) Uani 1 1 d .
C4 C 0.3799(3) 0.2725(2) -0.04747(16) 0.0526(5) Uani 1 1 d .
C18 C 0.2307(4) -0.1179(3) 0.20714(18) 0.0687(8) Uani 1 1 d .
H18A H 0.2914 -0.0614 0.1653 0.082 Uiso 1 1 calc R
H18B H 0.3015 -0.1701 0.2306 0.082 Uiso 1 1 calc R
C22 C 0.3620(3) 0.0726(3) 0.3489(2) 0.0718(8) Uani 1 1 d .
H22A H 0.4309 0.0124 0.3610 0.086 Uiso 1 1 calc R
H22B H 0.4154 0.1309 0.3058 0.086 Uiso 1 1 calc R
C2 C 0.2386(3) 0.1986(2) 0.09776(16) 0.0496(5) Uani 1 1 d .
C16 C -0.2242(4) 0.3539(3) 0.2972(2) 0.0790(9) Uani 1 1 d .
H16A H -0.2937 0.4053 0.2713 0.095 Uiso 1 1 calc R
H16B H -0.2892 0.2948 0.3361 0.095 Uiso 1 1 calc R
C8 C 0.5241(3) 0.4130(3) -0.29865(16) 0.0571(6) Uani 1 1 d .
C7 C 0.4174(3) 0.2956(3) -0.29308(17) 0.0607(6) Uani 1 1 d .
H7 H 0.3739 0.2483 -0.3454 0.073 Uiso 1 1 calc R
C21 C 0.1919(5) -0.2229(3) 0.4109(2) 0.0864(10) Uani 1 1 d .
H21A H 0.2075 -0.2797 0.3607 0.130 Uiso 1 1 calc R
H21B H 0.1410 -0.2735 0.4577 0.130 Uiso 1 1 calc R
H21C H 0.2948 -0.1727 0.4325 0.130 Uiso 1 1 calc R
C12 C -0.3319(3) 0.1624(3) 0.1517(2) 0.0716(8) Uani 1 1 d .
H12A H -0.3865 0.1011 0.1927 0.086 Uiso 1 1 calc R
H12B H -0.4041 0.2191 0.1373 0.086 Uiso 1 1 calc R
C6 C 0.3744(3) 0.2472(2) -0.21150(16) 0.0554(6) Uani 1 1 d .
H6 H 0.3027 0.1678 -0.2094 0.067 Uiso 1 1 calc R
C15 C -0.1759(4) 0.4554(3) 0.0902(3) 0.0876(10) Uani 1 1 d .
H15A H -0.2672 0.3985 0.0602 0.131 Uiso 1 1 calc R
H15B H -0.1197 0.5130 0.0485 0.131 Uiso 1 1 calc R
H15C H -0.2124 0.5050 0.1384 0.131 Uiso 1 1 calc R
C11 C 0.5645(5) 0.4688(3) -0.3886(2) 0.0841(10) Uani 1 1 d .
H11A H 0.5494 0.3996 -0.4346 0.126 Uiso 1 1 calc R
H11B H 0.6750 0.5152 -0.3869 0.126 Uiso 1 1 calc R
H11C H 0.4946 0.5269 -0.4011 0.126 Uiso 1 1 calc R
C23 C 0.3442(5) 0.1503(4) 0.4341(2) 0.0978(12) Uani 1 1 d .
H23A H 0.2699 0.2057 0.4238 0.147 Uiso 1 1 calc R
H23B H 0.4476 0.2023 0.4533 0.147 Uiso 1 1 calc R
H23C H 0.3039 0.0926 0.4795 0.147 Uiso 1 1 calc R
C19 C 0.0890(6) -0.2063(4) 0.1576(3) 0.1062(13) Uani 1 1 d .
H19A H 0.0267 -0.2611 0.1988 0.159 Uiso 1 1 calc R
H19B H 0.1280 -0.2590 0.1120 0.159 Uiso 1 1 calc R
H19C H 0.0224 -0.1550 0.1304 0.159 Uiso 1 1 calc R
C13 C -0.2987(5) 0.0895(4) 0.0678(3) 0.1078(13) Uani 1 1 d .
H13A H -0.2768 0.1479 0.0206 0.162 Uiso 1 1 calc R
H13B H -0.3912 0.0222 0.0509 0.162 Uiso 1 1 calc R
H13C H -0.2066 0.0516 0.0778 0.162 Uiso 1 1 calc R
C17 C -0.0919(6) 0.4425(4) 0.3525(3) 0.1269(17) Uani 1 1 d .
H17A H -0.0272 0.3919 0.3820 0.190 Uiso 1 1 calc R
H17B H -0.1386 0.4924 0.3965 0.190 Uiso 1 1 calc R
H17C H -0.0253 0.4999 0.3143 0.190 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'
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
C1 Pd P2 87.31(6)
C1 Pd P1 89.87(6)
P2 Pd P1 177.01(2)
C1 Pd Cl1 176.75(7)
P2 Pd Cl1 94.27(2)
P1 Pd Cl1 88.50(2)
C22 P2 C18 103.96(15)
C22 P2 C20 105.93(14)
C18 P2 C20 105.28(13)
C22 P2 Pd 110.95(11)
C18 P2 Pd 114.55(9)
C20 P2 Pd 115.19(9)
C14 P1 C12 105.36(14)
C14 P1 C16 105.60(15)
C12 P1 C16 104.18(16)
C14 P1 Pd 117.95(8)
C12 P1 Pd 108.63(10)
C16 P1 Pd 113.95(10)
C2 C1 Pd 173.3(2)
C10 C5 C6 117.9(2)
C10 C5 C4 121.5(2)
C6 C5 C4 120.5(2)
C8 C9 C10 121.0(2)
C21 C20 P2 115.6(2)
C15 C14 P1 115.7(2)
C9 C10 C5 120.9(2)
C4 C3 C2 177.2(3)
C3 C4 C5 173.7(3)
C19 C18 P2 113.3(2)
C23 C22 P2 113.7(2)
C1 C2 C3 174.2(2)
C17 C16 P1 113.4(3)
C9 C8 C7 118.3(2)
C9 C8 C11 120.7(3)
C7 C8 C11 120.9(3)
C6 C7 C8 121.2(2)
C13 C12 P1 113.0(2)
C7 C6 C5 120.6(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd C1 1.951(2)
Pd P2 2.3127(6)
Pd P1 2.3227(6)
Pd Cl1 2.3418(6)
P2 C22 1.819(3)
P2 C18 1.827(3)
P2 C20 1.827(2)
P1 C14 1.821(3)
P1 C12 1.822(3)
P1 C16 1.829(3)
C1 C2 1.199(3)
C5 C10 1.391(3)
C5 C6 1.393(3)
C5 C4 1.430(3)
C9 C8 1.378(4)
C9 C10 1.379(3)
C20 C21 1.522(4)
C14 C15 1.519(4)
C3 C4 1.200(3)
C3 C2 1.382(3)
C18 C19 1.510(5)
C22 C23 1.501(5)
C16 C17 1.501(5)
C8 C7 1.382(4)
C8 C11 1.517(3)
C7 C6 1.377(3)
C12 C13 1.494(5)
