#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:52:20 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178727 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/38/4083863.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_4083863
loop_
_publ_author_name
'Saha, Debajyoti'
'Verma, Ravi'
'Kumar, Devesh'
'Pathak, Shubhrodeep'
'Bhunya, Sourav'
'Sarkar, Amitabha'
_publ_section_title
;
 A “Hemilabile” Palladium--Carbon Bond: Characterization
 and Its Implication in Catalysis
;
_journal_name_full               Organometallics
_journal_page_first              140702101148002
_journal_paper_doi               10.1021/om5005435
_journal_year                    2014
_chemical_formula_sum            'C24 H22 Cl2 N P Pd'
_chemical_formula_weight         532.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.959(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6160(17)
_cell_length_b                   10.7894(13)
_cell_length_c                   14.6807(18)
_cell_measurement_reflns_used    6106
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.88
_cell_measurement_theta_min      2.23
_cell_volume                     2256.2(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'MERCURY 3.2'
_computing_publication_material  'ORTEP 3V.2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29418
_diffrn_reflns_theta_full        26.71
_diffrn_reflns_theta_max         26.71
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.8944
_exptl_absorpt_correction_T_min  0.8210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0355
_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)+(0.1000P)²+0.5107P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1298
_reflns_number_gt                3803
_reflns_number_total             4761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5005435_si_002.cif
_cod_data_source_block           TEST1
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/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      P2(1)/n
_cod_database_code               4083863
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Pd1 Pd 0.510870(17) 0.00914(2) 0.233009(18) 0.03533(13) Uani 1 1 d .
P1 P 0.40226(6) 0.15052(8) 0.24514(6) 0.0333(2) Uani 1 1 d .
Cl1 Cl 0.62490(8) -0.14572(11) 0.23194(9) 0.0653(3) Uani 1 1 d .
Cl2 Cl 0.41861(7) -0.13422(9) 0.28789(9) 0.0591(3) Uani 1 1 d .
C19 C 0.3488(2) 0.1361(3) 0.3446(2) 0.0400(8) Uani 1 1 d .
C13 C 0.3075(2) 0.1524(3) 0.1411(2) 0.0379(7) Uani 1 1 d .
C14 C 0.2845(3) 0.0428(4) 0.0909(3) 0.0489(9) Uani 1 1 d .
H14 H 0.3177 -0.0295 0.1103 0.059 Uiso 1 1 calc R
C20 C 0.4066(3) 0.1243(4) 0.4329(3) 0.0549(10) Uani 1 1 d .
H20 H 0.4709 0.1145 0.4397 0.066 Uiso 1 1 calc R
C15 C 0.2125(3) 0.0422(5) 0.0124(3) 0.0638(11) Uani 1 1 d .
H15 H 0.1972 -0.0308 -0.0213 0.077 Uiso 1 1 calc R
C16 C 0.1626(3) 0.1491(5) -0.0167(3) 0.0648(12) Uani 1 1 d .
H16 H 0.1138 0.1478 -0.0696 0.078 Uiso 1 1 calc R
C24 C 0.2530(3) 0.1483(4) 0.3359(3) 0.0542(10) Uani 1 1 d .
H24 H 0.2138 0.1569 0.2770 0.065 Uiso 1 1 calc R
C18 C 0.2570(3) 0.2585(4) 0.1113(3) 0.0524(9) Uani 1 1 d .
H18 H 0.2712 0.3322 0.1444 0.063 Uiso 1 1 calc R
C17 C 0.1844(3) 0.2549(5) 0.0312(3) 0.0672(12) Uani 1 1 d .
H17 H 0.1508 0.3267 0.0109 0.081 Uiso 1 1 calc R
C21 C 0.3684(3) 0.1271(5) 0.5113(3) 0.0700(13) Uani 1 1 d .
H21 H 0.4077 0.1215 0.5705 0.084 Uiso 1 1 calc R
C22 C 0.2734(4) 0.1379(5) 0.5023(3) 0.0790(14) Uani 1 1 d .
H22 H 0.2483 0.1386 0.5552 0.095 Uiso 1 1 calc R
C23 C 0.2151(3) 0.1480(5) 0.4145(3) 0.0755(14) Uani 1 1 d .
H23 H 0.1505 0.1545 0.4081 0.091 Uiso 1 1 calc R
C12 C 0.4462(2) 0.3090(3) 0.2578(2) 0.0403(8) Uani 1 1 d .
C8 C 0.5510(4) 0.4617(4) 0.2147(3) 0.0636(12) Uani 1 1 d .
H8 H 0.5969 0.4818 0.1823 0.076 Uiso 1 1 calc R
C7 C 0.5115(3) 0.3447(3) 0.2069(3) 0.0465(9) Uani 1 1 d .
C3 C 0.6012(3) 0.0850(4) 0.0978(3) 0.0639(12) Uani 1 1 d .
H3 H 0.6356 0.0131 0.0950 0.077 Uiso 1 1 calc R
C10 C 0.4572(4) 0.5167(4) 0.3222(4) 0.0622(13) Uani 1 1 d .
H10 H 0.4385 0.5748 0.3612 0.075 Uiso 1 1 calc R
C1 C 0.6770(3) 0.1688(5) 0.2622(4) 0.0710(13) Uani 1 1 d .
H1A H 0.7076 0.0912 0.2812 0.106 Uiso 1 1 calc R
H1B H 0.6556 0.2043 0.3137 0.106 Uiso 1 1 calc R
H1C H 0.7204 0.2244 0.2432 0.106 Uiso 1 1 calc R
C9 C 0.5212(4) 0.5494(4) 0.2718(3) 0.0669(13) Uani 1 1 d .
H9 H 0.5448 0.6297 0.2754 0.080 Uiso 1 1 calc R
C6 C 0.4423(4) 0.3388(5) -0.0023(3) 0.0818(16) Uani 1 1 d .
H6A H 0.4402 0.4125 0.0338 0.123 Uiso 1 1 calc R
H6B H 0.3811 0.3015 -0.0176 0.123 Uiso 1 1 calc R
H6C H 0.4615 0.3596 -0.0588 0.123 Uiso 1 1 calc R
C4 C 0.5499(4) 0.1452(5) 0.0226(3) 0.0734(14) Uani 1 1 d .
H4 H 0.5423 0.1205 -0.0393 0.088 Uiso 1 1 calc R
N1 N 0.5390(2) 0.2537(3) 0.1468(2) 0.0486(7) Uani 1 1 d .
C2 C 0.5950(3) 0.1475(4) 0.1824(3) 0.0499(9) Uani 1 1 d .
C5 C 0.5106(3) 0.2498(4) 0.0532(3) 0.0595(11) Uani 1 1 d .
C11 C 0.4193(3) 0.3978(3) 0.3164(3) 0.0515(9) Uani 1 1 d .
H11 H 0.3759 0.3773 0.3515 0.062 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
C2 Pd1 P1 91.43(11)
C2 Pd1 Cl2 178.47(11)
P1 Pd1 Cl2 87.06(4)
C2 Pd1 Cl1 91.69(11)
P1 Pd1 Cl1 175.52(4)
Cl2 Pd1 Cl1 89.81(4)
C19 P1 C13 107.09(15)
C19 P1 C12 101.79(17)
C13 P1 C12 105.06(15)
C19 P1 Pd1 116.60(11)
C13 P1 Pd1 111.18(11)
C12 P1 Pd1 114.08(12)
C24 C19 C20 119.1(3)
C24 C19 P1 121.9(3)
C20 C19 P1 118.7(3)
C18 C13 C14 119.2(3)
C18 C13 P1 121.9(3)
C14 C13 P1 118.9(3)
C15 C14 C13 119.7(4)
C19 C20 C21 120.1(4)
C14 C15 C16 120.4(4)
C17 C16 C15 120.2(4)
C19 C24 C23 120.6(4)
C13 C18 C17 119.7(4)
C16 C17 C18 120.8(4)
C22 C21 C20 120.7(4)
C21 C22 C23 119.8(4)
C22 C23 C24 119.8(4)
C7 C12 C11 117.4(3)
C7 C12 P1 118.3(3)
C11 C12 P1 124.3(3)
C7 C8 C9 119.1(5)
C8 C7 C12 122.2(4)
C8 C7 N1 120.3(4)
C12 C7 N1 117.5(3)
C4 C3 C2 110.4(4)
C9 C10 C11 121.1(4)
C10 C9 C8 119.7(4)
C3 C4 C5 108.7(4)
C5 N1 C2 111.5(3)
C5 N1 C7 125.8(4)
C2 N1 C7 122.4(3)
C3 C2 N1 101.6(4)
C3 C2 C1 123.8(4)
N1 C2 C1 117.0(4)
C3 C2 Pd1 97.1(3)
N1 C2 Pd1 110.7(2)
C1 C2 Pd1 104.7(3)
N1 C5 C4 107.5(4)
N1 C5 C6 123.7(4)
C4 C5 C6 128.6(4)
C10 C11 C12 120.4(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 C2 2.169(4)
Pd1 P1 2.2373(9)
Pd1 Cl2 2.3125(10)
Pd1 Cl1 2.3626(10)
P1 C19 1.810(4)
P1 C13 1.817(3)
P1 C12 1.821(4)
C19 C24 1.383(5)
C19 C20 1.385(5)
C13 C18 1.380(5)
C13 C14 1.394(5)
C14 C15 1.376(5)
C20 C21 1.386(6)
C15 C16 1.380(7)
C16 C17 1.341(6)
C24 C23 1.388(6)
C18 C17 1.396(5)
C21 C22 1.370(7)
C22 C23 1.381(7)
C12 C7 1.391(5)
C12 C11 1.402(5)
C8 C7 1.383(6)
C8 C9 1.398(7)
C7 N1 1.437(5)
C3 C4 1.353(7)
C3 C2 1.434(6)
C10 C9 1.363(7)
C10 C11 1.392(6)
C1 C2 1.494(6)
C6 C5 1.489(6)
C4 C5 1.386(6)
N1 C5 1.344(5)
N1 C2 1.437(5)
