#------------------------------------------------------------------------------
#$Date: 2018-09-09 00:18:38 +0300 (Sun, 09 Sep 2018) $
#$Revision: 210593 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/39/7103983.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_7103983
loop_
_publ_author_name
'Albert, Joan'
'Cadena, J. Magali'
'González, Asensio'
'Granell, Jaume'
'Solans, Xavier'
'Font-Bardia, Mercè'
_publ_section_title
;
 The first NH aldimine organometallic compound. Isolation and crystal structure
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   4
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              528
_journal_page_last               529
_journal_paper_doi               10.1039/b211808d
_journal_year                    2003
_chemical_formula_sum            'C28 H27 Cl N P Pd'
_chemical_formula_weight         550.33
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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
_cell_angle_beta                 114.2640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1670(10)
_cell_length_b                   24.9410(10)
_cell_length_c                   10.6240(10)
_cell_measurement_reflns_used    8954
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      3
_cell_volume                     2456.0(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.498
_diffrn_measured_fraction_theta_max 0.498
_diffrn_measurement_device_type  'Marresearch 2300'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10751
_diffrn_reflns_theta_full        31.49
_diffrn_reflns_theta_max         31.49
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.946
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       0.0138(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         4209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1030P)²+2.2441P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1480
_reflns_number_gt                3524
_reflns_number_total             4209
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211808d.txt
_cod_data_source_block           jgfm95a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.1030P)^2^+2.2441P] 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^)+(0.1030P)^2^+2.2441P] 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      P21/c
_cod_database_code               7103983
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.27886(4) 0.059865(10) 0.10394(3) 0.0328(2) Uani 1 d . . .
P2 P 0.17402(15) 0.14091(3) 0.08874(10) 0.0312(4) Uani 1 d . . .
Cl Cl 0.42786(17) 0.08700(4) -0.01520(12) 0.0456(4) Uani 1 d . . .
N N 0.3732(6) -0.01513(12) 0.1323(4) 0.0413(13) Uani 1 d . . .
C1 C 0.3902(7) -0.04894(15) 0.2277(5) 0.0391(15) Uani 1 d . . .
C2 C 0.3416(6) -0.03960(14) 0.3369(4) 0.0351(13) Uani 1 d . . .
C3 C 0.4072(7) -0.06617(15) 0.4640(5) 0.0408(16) Uani 1 d . . .
C4 C 0.5180(8) -0.1091(2) 0.4874(6) 0.0592(18) Uani 1 d . . .
H4 H 0.5911 -0.0962 0.4598 0.071 Uiso 1 calc R . .
H4A H 0.4727 -0.1402 0.4339 0.071 Uiso 1 calc R . .
H4B H 0.5612 -0.1184 0.5836 0.071 Uiso 1 calc R . .
C5 C 0.3683(7) -0.05210(18) 0.5704(5) 0.0460(17) Uani 1 d . . .
C6 C 0.2668(7) -0.01365(17) 0.5550(5) 0.0497(17) Uani 1 d . . .
C7 C 0.2295(9) 0.0022(2) 0.6737(6) 0.068(2) Uani 1 d . . .
H7 H 0.1400 0.0215 0.6389 0.081 Uiso 1 calc R . .
H7A H 0.3046 0.0245 0.7368 0.081 Uiso 1 calc R . .
H7B H 0.2201 -0.0295 0.7208 0.081 Uiso 1 calc R . .
C8 C 0.1965(8) 0.01056(16) 0.4268(5) 0.0470(17) Uani 1 d . . .
C9 C 0.2310(6) -0.00173(14) 0.3162(4) 0.0360(14) Uani 1 d . . .
C10 C 0.1474(6) 0.02238(15) 0.1788(5) 0.0389(14) Uani 1 d . . .
H10 H 0.0793 0.0481 0.1860 0.021(10) Uiso 1 calc R . .
H10A H 0.0931 -0.0055 0.1149 0.026 Uiso 1 calc R . .
C11 C 0.2932(7) 0.19768(14) 0.1655(4) 0.0333(15) Uani 1 d . . .
C12 C 0.4358(9) 0.1951(2) 0.1882(6) 0.0534(19) Uani 1 d . . .
C13 C 0.5280(9) 0.2375(3) 0.2512(8) 0.070(2) Uani 1 d . . .
H13 H 0.6250 0.2354 0.2675 0.083 Uiso 1 calc R . .
C14 C 0.4754(12) 0.2826(2) 0.2893(7) 0.073(3) Uani 1 d . . .
C15 C 0.3348(11) 0.2860(2) 0.2669(7) 0.063(2) Uani 1 d . . .
C16 C 0.2447(9) 0.24391(17) 0.2066(6) 0.0493(18) Uani 1 d . . .
C17 C 0.0629(6) 0.15853(13) -0.0892(4) 0.0307(13) Uani 1 d . . .
C18 C -0.0010(7) 0.20894(15) -0.1274(4) 0.0408(14) Uani 1 d . . .
C28 C 0.0960(9) 0.15050(17) 0.3106(5) 0.0394(17) Uani 1 d . . .
C19 C -0.0972(7) 0.21875(17) -0.2605(5) 0.0507(16) Uani 1 d . . .
C20 C -0.1335(7) 0.17873(19) -0.3580(5) 0.0471(16) Uani 1 d . . .
C21 C -0.0705(7) 0.12933(17) -0.3239(4) 0.0443(15) Uani 1 d . . .
C22 C 0.0271(7) 0.11884(15) -0.1901(4) 0.0431(15) Uani 1 d . . .
C23 C 0.0460(6) 0.14478(14) 0.1677(4) 0.0298(14) Uani 1 d . . .
C24 C -0.0984(8) 0.13549(17) 0.0931(6) 0.0433(17) Uani 1 d . . .
C25 C -0.1942(7) 0.13207(19) 0.1567(6) 0.0506(16) Uani 1 d . . .
H25 H -0.2921 0.1261 0.1046 0.061 Uiso 1 calc R . .
C26 C -0.1411(10) 0.13771(19) 0.2980(7) 0.051(2) Uani 1 d . . .
C27 C 0.0022(9) 0.14723(18) 0.3742(6) 0.0466(18) Uani 1 d . . .
H1N H 0.418(5) -0.0246(15) 0.076(4) 0.023(10) Uiso 1 d . . .
H1 H 0.438(6) -0.084(2) 0.232(5) 0.042(13) Uiso 1 d . . .
H5 H 0.414(7) -0.069(2) 0.663(6) 0.057(16) Uiso 1 d . . .
H8 H 0.124(6) 0.0360(17) 0.412(4) 0.025(10) Uiso 1 d . . .
H12 H 0.467(6) 0.160(2) 0.161(5) 0.054(15) Uiso 1 d . . .
H14 H 0.546(7) 0.308(2) 0.338(6) 0.060(16) Uiso 1 d . . .
H15 H 0.280(9) 0.322(3) 0.276(8) 0.10(2) Uiso 1 d . . .
H16 H 0.145(6) 0.2471(16) 0.198(4) 0.022(12) Uiso 1 d . . .
H18 H 0.030(7) 0.237(2) -0.063(6) 0.050(14) Uiso 1 d . . .
H19 H -0.136(6) 0.255(2) -0.294(5) 0.047(14) Uiso 1 d . . .
H20 H -0.201(6) 0.1822(17) -0.447(5) 0.034(12) Uiso 1 d . . .
H21 H -0.090(8) 0.100(3) -0.392(7) 0.08(2) Uiso 1 d . . .
H22 H 0.067(6) 0.0873(19) -0.168(4) 0.032(11) Uiso 1 d . . .
H24 H -0.130(6) 0.1315(18) 0.009(5) 0.036(12) Uiso 1 d . . .
H26 H -0.197(7) 0.1350(19) 0.342(5) 0.042(14) Uiso 1 d . . .
H27 H 0.030(7) 0.148(2) 0.466(7) 0.067(17) Uiso 1 d . . .
H28 H 0.188(6) 0.1558(16) 0.357(5) 0.017(12) Uiso 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'
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
C10 Pd1 N 82.39(17) . . ?
C10 Pd1 P2 94.15(12) . . ?
N Pd1 P2 175.51(10) . . ?
C10 Pd1 Cl 167.57(12) . . ?
N Pd1 Cl 88.67(12) . . ?
P2 Pd1 Cl 95.17(4) . . ?
C17 P2 C23 102.2(2) . . ?
C17 P2 C11 107.03(18) . . ?
C23 P2 C11 102.8(2) . . ?
C17 P2 Pd1 111.40(12) . . ?
C23 P2 Pd1 114.88(12) . . ?
C11 P2 Pd1 117.1(2) . . ?
C1 N Pd1 128.2(3) . . ?
C1 N H1N 114(3) . . ?
Pd1 N H1N 117(2) . . ?
N C1 C2 123.3(4) . . ?
N C1 H1 122(3) . . ?
C2 C1 H1 115(3) . . ?
C3 C2 C9 119.8(4) . . ?
C3 C2 C1 120.7(5) . . ?
C9 C2 C1 119.5(4) . . ?
C5 C3 C2 118.9(5) . . ?
C5 C3 C4 119.5(4) . . ?
C2 C3 C4 121.6(4) . . ?
C3 C4 H4 109.5 . . ?
C3 C4 H4A 109.5 . . ?
H4 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C6 C5 C3 122.2(5) . . ?
C6 C5 H5 116(3) . . ?
C3 C5 H5 122(4) . . ?
C5 C6 C8 118.7(5) . . ?
C5 C6 C7 121.2(5) . . ?
C8 C6 C7 120.0(6) . . ?
C6 C7 H7 109.5 . . ?
C6 C7 H7A 109.5 . . ?
H7 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C8 C9 121.7(5) . . ?
C6 C8 H8 121(2) . . ?
C9 C8 H8 118(2) . . ?
C8 C9 C2 118.4(4) . . ?
C8 C9 C10 120.0(5) . . ?
C2 C9 C10 121.4(4) . . ?
C9 C10 Pd1 111.6(4) . . ?
C9 C10 H10 109.3 . . ?
Pd1 C10 H10 109.3 . . ?
C9 C10 H10A 109.3 . . ?
Pd1 C10 H10A 109.3 . . ?
H10 C10 H10A 108.0 . . ?
C12 C11 C16 118.0(5) . . ?
C12 C11 P2 120.2(3) . . ?
C16 C11 P2 121.8(6) . . ?
C11 C12 C13 120.3(6) . . ?
C11 C12 H12 115(3) . . ?
C13 C12 H12 125(3) . . ?
C14 C13 C12 119.9(8) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C15 C14 C13 120.6(6) . . ?
C15 C14 H14 125(4) . . ?
C13 C14 H14 115(4) . . ?
C14 C15 C16 119.5(6) . . ?
C14 C15 H15 126(4) . . ?
C16 C15 H15 114(5) . . ?
C15 C16 C11 121.8(8) . . ?
C15 C16 H16 117(3) . . ?
C11 C16 H16 121(3) . . ?
C22 C17 C18 118.2(4) . . ?
C22 C17 P2 118.9(3) . . ?
C18 C17 P2 122.5(3) . . ?
C19 C18 C17 120.7(4) . . ?
C19 C18 H18 120(3) . . ?
C17 C18 H18 119(3) . . ?
C27 C28 C23 120.7(7) . . ?
C27 C28 H28 122(3) . . ?
C23 C28 H28 117(3) . . ?
C18 C19 C20 120.3(4) . . ?
C18 C19 H19 123(3) . . ?
C20 C19 H19 116(3) . . ?
C21 C20 C19 120.2(5) . . ?
C21 C20 H20 116(3) . . ?
C19 C20 H20 124(3) . . ?
C20 C21 C22 120.2(4) . . ?
C20 C21 H21 123(4) . . ?
C22 C21 H21 117(4) . . ?
C21 C22 C17 120.4(4) . . ?
C21 C22 H22 120(3) . . ?
C17 C22 H22 119(3) . . ?
C24 C23 C28 118.0(5) . . ?
C24 C23 P2 121.6(3) . . ?
C28 C23 P2 119.9(5) . . ?
C23 C24 C25 121.6(5) . . ?
C23 C24 H24 120(4) . . ?
C25 C24 H24 118(4) . . ?
C26 C25 C24 118.8(6) . . ?
C26 C25 H25 120.6 . . ?
C24 C25 H25 120.6 . . ?
C27 C26 C25 120.6(6) . . ?
C27 C26 H26 118(4) . . ?
C25 C26 H26 122(4) . . ?
C26 C27 C28 120.2(6) . . ?
C26 C27 H27 116(4) . . ?
C28 C27 H27 124(4) . . ?
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 C10 2.041(5) . ?
Pd1 N 2.067(3) . ?
Pd1 P2 2.2597(10) . ?
Pd1 Cl 2.4354(12) . ?
P2 C17 1.813(4) . ?
P2 C23 1.817(5) . ?
P2 C11 1.824(5) . ?
N C1 1.275(5) . ?
N H1N 0.92(4) . ?
C1 C2 1.454(6) . ?
C1 H1 0.99(5) . ?
C2 C3 1.403(6) . ?
C2 C9 1.415(7) . ?
C3 C5 1.387(7) . ?
C3 C4 1.499(8) . ?
C4 H4 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C5 C6 1.368(8) . ?
C5 H5 0.99(6) . ?
C6 C8 1.389(7) . ?
C6 C7 1.511(7) . ?
C7 H7 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C8 C9 1.392(6) . ?
C8 H8 0.94(5) . ?
C9 C10 1.481(6) . ?
C10 H10 0.9700 . ?
C10 H10A 0.9700 . ?
C11 C12 1.370(8) . ?
C11 C16 1.393(7) . ?
C12 C13 1.389(8) . ?
C12 H12 1.02(5) . ?
C13 C14 1.377(10) . ?
C13 H13 0.9300 . ?
C14 C15 1.352(10) . ?
C14 H14 0.94(6) . ?
C15 C16 1.367(9) . ?
C15 H15 1.08(8) . ?
C16 H16 0.98(6) . ?
C17 C22 1.393(5) . ?
C17 C18 1.397(5) . ?
C18 C19 1.371(7) . ?
C18 H18 0.93(5) . ?
C28 C27 1.378(8) . ?
C28 C23 1.397(6) . ?
C28 H28 0.87(5) . ?
C19 C20 1.375(7) . ?
C19 H19 0.99(5) . ?
C20 C21 1.367(7) . ?
C20 H20 0.91(5) . ?
C21 C22 1.383(7) . ?
C21 H21 1.00(7) . ?
C22 H22 0.87(5) . ?
C23 C24 1.372(8) . ?
C24 C25 1.398(7) . ?
C24 H24 0.82(5) . ?
C25 C26 1.377(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.366(9) . ?
C26 H26 0.87(6) . ?
C27 H27 0.90(6) . ?
