#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:53:07 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179133 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/95/4309531.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_4309531
loop_
_publ_author_name
'Brandon L. Dietrich'
'Jonathan Egbert'
'Aimee M. Morris'
'Mark Wicholas'
'Oren P. Anderson'
'Susie M. Miller'
_publ_section_title
;
Cd(II), Zn(II), and Pd(II) Complexes of an Isoindoline Pincer Ligand:
Consequences of Steric Crowding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6476
_journal_page_last               6481
_journal_paper_doi               10.1021/ic0506916
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C24 H24 Cl N5 O Pd'
_chemical_formula_weight         540.33
_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                73.811(2)
_cell_angle_beta                 79.324(2)
_cell_angle_gamma                79.795(2)
_cell_formula_units_Z            2
_cell_length_a                   7.4036(8)
_cell_length_b                   11.0386(11)
_cell_length_c                   14.1390(15)
_cell_measurement_reflns_used    4179
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.75
_cell_volume                     1080.8(2)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10050
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    1.010
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.540
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       0.062(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         5157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0621P)²+0.5595P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                4633
_reflns_number_total             5157
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0506916si20050503_013101.cif
_cod_data_source_block           mw109m
_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 
;
_cod_database_code               4309531
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.36271(3) 1.252749(19) 0.317569(15) 0.01579(11) Uani 1 1 d . . .
Cl Cl 0.51410(12) 1.43686(7) 0.26481(6) 0.02649(19) Uani 1 1 d . . .
N1 N 0.3019(3) 1.0778(2) 0.35259(19) 0.0175(5) Uani 1 1 d . . .
N2 N 0.3857(4) 1.0348(2) 0.1893(2) 0.0213(5) Uani 1 1 d . . .
N3 N 0.3371(4) 1.2621(2) 0.16644(19) 0.0191(5) Uani 1 1 d . . .
N4 N 0.2405(4) 1.0265(2) 0.53194(19) 0.0194(5) Uani 1 1 d . . .
N5 N 0.2524(4) 1.1484(3) 0.6340(2) 0.0189(5) Uani 1 1 d . . .
H5A H 0.207(7) 1.095(5) 0.669(4) 0.048(14) Uiso 1 1 d . . .
C1 C 0.3238(4) 1.0067(3) 0.2838(2) 0.0175(6) Uani 1 1 d . . .
C2 C 0.2672(4) 0.8794(3) 0.3366(2) 0.0186(6) Uani 1 1 d . . .
C3 C 0.2488(4) 0.7771(3) 0.3016(2) 0.0228(6) Uani 1 1 d . . .
H3A H 0.2792 0.7790 0.2329 0.027 Uiso 1 1 calc R . .
C4 C 0.1839(5) 0.6717(3) 0.3712(3) 0.0254(7) Uani 1 1 d . . .
H4B H 0.1694 0.6002 0.3496 0.030 Uiso 1 1 calc R . .
C5 C 0.1401(4) 0.6690(3) 0.4714(3) 0.0247(7) Uani 1 1 d . . .
H5B H 0.0966 0.5955 0.5172 0.030 Uiso 1 1 calc R . .
C6 C 0.1584(4) 0.7720(3) 0.5067(2) 0.0223(6) Uani 1 1 d . . .
H6A H 0.1284 0.7702 0.5753 0.027 Uiso 1 1 calc R . .
C7 C 0.2224(4) 0.8771(3) 0.4369(2) 0.0187(6) Uani 1 1 d . . .
C8 C 0.2537(4) 1.0013(3) 0.4466(2) 0.0172(5) Uani 1 1 d . . .
C9 C 0.2825(4) 1.1411(3) 0.5377(2) 0.0174(6) Uani 1 1 d . . .
C10 C 0.2769(4) 1.2491(3) 0.6648(2) 0.0201(6) Uani 1 1 d . . .
C11 C 0.3403(4) 1.3508(3) 0.5931(2) 0.0217(6) Uani 1 1 d . . .
H11A H 0.3592 1.4237 0.6113 0.026 Uiso 1 1 calc R . .
C12 C 0.3767(4) 1.3470(3) 0.4941(2) 0.0204(6) Uani 1 1 d . . .
H12A H 0.4243 1.4174 0.4461 0.025 Uiso 1 1 calc R . .
C13 C 0.3466(4) 1.2439(3) 0.4614(2) 0.0172(5) Uani 1 1 d . . .
C14 C 0.3020(5) 1.3765(3) 0.0997(2) 0.0222(6) Uani 1 1 d . . .
C15 C 0.3621(5) 1.3915(3) -0.0016(2) 0.0266(7) Uani 1 1 d . . .
H15A H 0.3375 1.4717 -0.0473 0.032 Uiso 1 1 calc R . .
C16 C 0.4584(5) 1.2882(3) -0.0354(2) 0.0282(7) Uani 1 1 d . . .
H16A H 0.5127 1.2990 -0.1031 0.034 Uiso 1 1 calc R . .
C17 C 0.4742(5) 1.1697(3) 0.0305(2) 0.0246(6) Uani 1 1 d . . .
H17A H 0.5328 1.0970 0.0078 0.030 Uiso 1 1 calc R . .
C18 C 0.4032(4) 1.1573(3) 0.1313(2) 0.0210(6) Uani 1 1 d . . .
C19 C 0.2339(5) 1.2420(3) 0.7736(2) 0.0284(7) Uani 1 1 d . . .
H19A H 0.1914 1.1600 0.8095 0.043 Uiso 1 1 calc R . .
H19B H 0.1364 1.3113 0.7848 0.043 Uiso 1 1 calc R . .
H19C H 0.3458 1.2500 0.7979 0.043 Uiso 1 1 calc R . .
O1 O 0.1334(5) 0.9498(2) 0.79238(19) 0.0437(7) Uani 1 1 d . . .
C20 C 0.1841(5) 1.4841(3) 0.1370(3) 0.0286(7) Uani 1 1 d . . .
H20A H 0.1550 1.4575 0.2097 0.043 Uiso 1 1 calc R . .
H20B H 0.0688 1.5069 0.1077 0.043 Uiso 1 1 calc R . .
H20C H 0.2518 1.5579 0.1179 0.043 Uiso 1 1 calc R . .
C21 C 0.0550(6) 0.9511(3) 0.8917(3) 0.0320(8) Uani 1 1 d . . .
H21A H -0.0701 1.0010 0.8929 0.038 Uiso 1 1 calc R . .
H21B H 0.1336 0.9909 0.9208 0.038 Uiso 1 1 calc R . .
C22 C 0.0426(5) 0.8144(3) 0.9515(3) 0.0291(7) Uani 1 1 d . . .
H22A H -0.0881 0.7980 0.9705 0.035 Uiso 1 1 calc R . .
H22B H 0.1013 0.7950 1.0124 0.035 Uiso 1 1 calc R . .
C23 C 0.1488(5) 0.7357(3) 0.8799(3) 0.0277(7) Uani 1 1 d . . .
H23A H 0.2804 0.7112 0.8901 0.033 Uiso 1 1 calc R . .
H23B H 0.0920 0.6580 0.8884 0.033 Uiso 1 1 calc R . .
C24 C 0.1309(5) 0.8264(3) 0.7781(3) 0.0288(7) Uani 1 1 d . . .
H24A H 0.2358 0.8059 0.7280 0.035 Uiso 1 1 calc R . .
H24B H 0.0133 0.8223 0.7561 0.035 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'
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'
O O 0.0106 0.0060 '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 Pd C13 89.88(11) . . ?
N1 Pd N3 87.16(10) . . ?
C13 Pd N3 171.65(11) . . ?
N1 Pd Cl 165.13(8) . . ?
C13 Pd Cl 93.65(9) . . ?
N3 Pd Cl 91.19(7) . . ?
C1 N1 C8 108.9(2) . . ?
C1 N1 Pd 123.0(2) . . ?
C8 N1 Pd 127.7(2) . . ?
C1 N2 C18 124.3(3) . . ?
C18 N3 C14 118.6(3) . . ?
C18 N3 Pd 118.4(2) . . ?
C14 N3 Pd 120.8(2) . . ?
C8 N4 C9 120.7(3) . . ?
C10 N5 C9 125.1(3) . . ?
N2 C1 N1 130.4(3) . . ?
N2 C1 C2 121.5(3) . . ?
N1 C1 C2 108.1(2) . . ?
C7 C2 C3 121.5(3) . . ?
C7 C2 C1 107.0(2) . . ?
C3 C2 C1 131.5(3) . . ?
C2 C3 C4 117.3(3) . . ?
C5 C4 C3 121.2(3) . . ?
C4 C5 C6 121.5(3) . . ?
C7 C6 C5 117.1(3) . . ?
C6 C7 C2 121.4(3) . . ?
C6 C7 C8 131.8(3) . . ?
C2 C7 C8 106.8(3) . . ?
N4 C8 N1 128.5(3) . . ?
N4 C8 C7 122.7(3) . . ?
N1 C8 C7 108.8(2) . . ?
N5 C9 N4 110.4(3) . . ?
N5 C9 C13 119.6(3) . . ?
N4 C9 C13 130.0(3) . . ?
N5 C10 C11 117.2(3) . . ?
N5 C10 C19 118.1(3) . . ?
C11 C10 C19 124.7(3) . . ?
C10 C11 C12 119.9(3) . . ?
C11 C12 C13 123.1(3) . . ?
C12 C13 C9 114.9(3) . . ?
C12 C13 Pd 122.0(2) . . ?
C9 C13 Pd 122.7(2) . . ?
N3 C14 C15 121.1(3) . . ?
N3 C14 C20 118.5(3) . . ?
C15 C14 C20 120.3(3) . . ?
C16 C15 C14 119.5(3) . . ?
C17 C16 C15 119.1(3) . . ?
C16 C17 C18 119.4(3) . . ?
N3 C18 N2 122.4(3) . . ?
N3 C18 C17 120.7(3) . . ?
N2 C18 C17 116.5(3) . . ?
C21 O1 C24 109.2(3) . . ?
O1 C21 C22 108.1(3) . . ?
C21 C22 C23 103.7(3) . . ?
C24 C23 C22 103.0(3) . . ?
O1 C24 C23 104.4(3) . . ?
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
Pd N1 1.967(2) . ?
Pd C13 1.990(3) . ?
Pd N3 2.152(3) . ?
Pd Cl 2.3654(8) . ?
N1 C1 1.382(4) . ?
N1 C8 1.383(4) . ?
N2 C1 1.297(4) . ?
N2 C18 1.386(4) . ?
N3 C18 1.362(4) . ?
N3 C14 1.365(4) . ?
N4 C8 1.295(4) . ?
N4 C9 1.382(4) . ?
N5 C10 1.352(4) . ?
N5 C9 1.362(4) . ?
C1 C2 1.488(4) . ?
C2 C7 1.389(4) . ?
C2 C3 1.391(4) . ?
C3 C4 1.392(5) . ?
C4 C5 1.388(5) . ?
C5 C6 1.398(4) . ?
C6 C7 1.387(4) . ?
C7 C8 1.477(4) . ?
C9 C13 1.413(4) . ?
C10 C11 1.373(4) . ?
C10 C19 1.496(4) . ?
C11 C12 1.386(4) . ?
C12 C13 1.407(4) . ?
C14 C15 1.392(4) . ?
C14 C20 1.503(5) . ?
C15 C16 1.388(5) . ?
C16 C17 1.379(5) . ?
C17 C18 1.402(4) . ?
O1 C21 1.420(4) . ?
O1 C24 1.435(4) . ?
C21 C22 1.519(5) . ?
C22 C23 1.533(5) . ?
C23 C24 1.521(5) . ?
