#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:00:29 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180055 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/01/7050164.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_7050164
loop_
_publ_author_name
'Gülay Gümüş'
'Vefa Ahsen'
'Colette Lebrun'
'Dominique Luneau'
'Jacques Pécaut'
_publ_section_title
;
 Unprecedented tubular channels assemblies afforded by
 alkyl-substituted oxamide oxime metal complexes
;
_journal_issue                   2
_journal_name_full               'New J. Chem.'
_journal_page_first              177
_journal_page_last               179
_journal_paper_doi               10.1039/b307783g
_journal_volume                  28
_journal_year                    2004
_chemical_formula_sum            'C28 H58 N8 O4 Pd'
_chemical_formula_weight         677.22
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   27.8737(19)
_cell_length_b                   27.8737(19)
_cell_length_c                   12.4102(13)
_cell_measurement_temperature    298(2)
_cell_volume                     8350.2(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.885
_diffrn_measured_fraction_theta_max 0.885
_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  0.0652
_diffrn_reflns_av_sigmaI/netI    0.1911
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11101
_diffrn_reflns_theta_full        29.60
_diffrn_reflns_theta_max         29.60
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.651
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         4622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.651
_refine_ls_R_factor_all          0.1684
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.004
_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+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1504
_reflns_number_gt                1752
_reflns_number_total             4622
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b307783g.txt
_cod_data_source_block           gulaypd
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7050164
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.5000 0.5000 0.0000 0.0527(2) Uani 1 2 d S . .
O1 O 0.41985(11) 0.40604(11) -0.1238(2) 0.0673(9) Uani 1 1 d . . .
O2 O 0.48357(13) 0.53195(13) 0.2173(3) 0.0861(11) Uani 1 1 d . . .
H2A H 0.5153 0.5553 0.2006 0.129 Uiso 1 1 calc R . .
N1 N 0.42778(14) 0.43370(14) -0.0309(3) 0.0571(9) Uani 1 1 d . . .
N2 N 0.45978(15) 0.49367(15) 0.1341(3) 0.0633(10) Uani 1 1 d . . .
N3 N 0.33765(15) 0.37353(15) 0.0368(3) 0.0725(11) Uani 1 1 d . . .
H3A H 0.3243 0.3539 0.0940 0.087 Uiso 1 1 calc R . .
N4 N 0.37283(17) 0.44209(18) 0.2233(3) 0.0853(13) Uani 1 1 d . . .
H4A H 0.3401 0.4142 0.2144 0.102 Uiso 1 1 calc R . .
C1 C 0.38989(18) 0.41851(17) 0.0436(4) 0.0579(12) Uani 1 1 d . . .
C2 C 0.40885(19) 0.45390(19) 0.1415(4) 0.0603(12) Uani 1 1 d . . .
C11 C 0.3032(2) 0.3563(3) -0.0571(5) 0.099(2) Uani 1 1 d . . .
H11A H 0.2670 0.3255 -0.0386 0.119 Uiso 1 1 calc R . .
H11B H 0.3193 0.3435 -0.1112 0.119 Uiso 1 1 calc R . .
C12 C 0.2967(3) 0.4033(3) -0.1034(7) 0.143(3) Uani 1 1 d . . .
H12A H 0.2821 0.4165 -0.0472 0.172 Uiso 1 1 calc R . .
H12B H 0.3333 0.4335 -0.1216 0.172 Uiso 1 1 calc R . .
C13 C 0.2622(4) 0.3908(5) -0.1962(9) 0.216(5) Uani 1 1 d . . .
H13A H 0.2255 0.3608 -0.1781 0.259 Uiso 1 1 calc R . .
H13B H 0.2767 0.3774 -0.2525 0.259 Uiso 1 1 calc R . .
C14 C 0.2565(6) 0.4389(7) -0.2419(12) 0.266(8) Uani 1 1 d . . .
H14A H 0.2390 0.4509 -0.1892 0.319 Uiso 1 1 calc R . .
H14B H 0.2928 0.4700 -0.2583 0.319 Uiso 1 1 calc R . .
C15 C 0.2251(13) 0.4215(10) -0.333(2) 0.408(17) Uani 1 1 d . . .
H15A H 0.2463 0.4161 -0.3892 0.490 Uiso 1 1 calc R . .
H15B H 0.1926 0.3859 -0.3190 0.490 Uiso 1 1 calc R . .
C16 C 0.2103(11) 0.4527(11) -0.3668(17) 0.372(14) Uani 1 1 d . . .
H16A H 0.1887 0.4375 -0.4310 0.558 Uiso 1 1 calc R . .
H16B H 0.2422 0.4879 -0.3831 0.558 Uiso 1 1 calc R . .
H16C H 0.1882 0.4575 -0.3131 0.558 Uiso 1 1 calc R . .
C21 C 0.3835(3) 0.4717(3) 0.3254(5) 0.125(3) Uani 1 1 d . . .
H21A H 0.3828 0.4470 0.3813 0.150 Uiso 1 1 calc R . .
H21B H 0.4211 0.5027 0.3223 0.150 Uiso 1 1 calc R . .
C22 C 0.3542(6) 0.4900(7) 0.3561(11) 0.359(13) Uani 1 1 d . . .
H22A H 0.3788 0.5298 0.3553 0.431 Uiso 1 1 calc R . .
H22B H 0.3480 0.4797 0.4316 0.431 Uiso 1 1 calc R . .
C23 C 0.3040(4) 0.4832(4) 0.3215(9) 0.199(4) Uani 1 1 d . . .
H23A H 0.2745 0.4502 0.3552 0.239 Uiso 1 1 calc R . .
H23B H 0.3012 0.4768 0.2444 0.239 Uiso 1 1 calc R . .
C24 C 0.2939(5) 0.5298(5) 0.3437(12) 0.236(6) Uani 1 1 d . . .
H24A H 0.3203 0.5618 0.3026 0.283 Uiso 1 1 calc R . .
H24B H 0.3008 0.5393 0.4195 0.283 Uiso 1 1 calc R . .
C25 C 0.2385(6) 0.5182(6) 0.3176(13) 0.260(7) Uani 1 1 d . . .
H25A H 0.2312 0.5074 0.2425 0.312 Uiso 1 1 calc R . .
H25B H 0.2123 0.4869 0.3605 0.312 Uiso 1 1 calc R . .
C26 C 0.2288(7) 0.5626(6) 0.3349(15) 0.378(12) Uani 1 1 d . . .
H26A H 0.1913 0.5514 0.3154 0.568 Uiso 1 1 calc R . .
H26B H 0.2538 0.5936 0.2914 0.568 Uiso 1 1 calc R . .
H26C H 0.2346 0.5729 0.4095 0.568 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'
O O 0.0106 0.0060 '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
N2 Pd N2 180.0(2) . 10_665 ?
N2 Pd N1 79.14(15) . . ?
N2 Pd N1 100.86(15) 10_665 . ?
N2 Pd N1 100.86(15) . 10_665 ?
N2 Pd N1 79.14(15) 10_665 10_665 ?
N1 Pd N1 180.000(1) . 10_665 ?
C1 N1 O1 123.2(3) . . ?
C1 N1 Pd 116.6(3) . . ?
O1 N1 Pd 120.2(3) . . ?
C2 N2 O2 120.1(4) . . ?
C2 N2 Pd 117.9(3) . . ?
O2 N2 Pd 121.9(3) . . ?
C1 N3 C11 125.9(4) . . ?
C2 N4 C21 126.8(4) . . ?
N1 C1 N3 124.8(4) . . ?
N1 C1 C2 113.7(4) . . ?
N3 C1 C2 121.4(4) . . ?
N2 C2 N4 128.7(4) . . ?
N2 C2 C1 112.6(4) . . ?
N4 C2 C1 118.6(4) . . ?
N3 C11 C12 111.5(6) . . ?
C13 C12 C11 116.8(9) . . ?
C12 C13 C14 115.9(11) . . ?
C15 C14 C13 109.0(18) . . ?
C16 C15 C14 115(3) . . ?
C22 C21 N4 121.2(8) . . ?
C21 C22 C23 133.6(10) . . ?
C22 C23 C24 116.4(11) . . ?
C23 C24 C25 114.2(11) . . ?
C26 C25 C24 115.0(14) . . ?
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 N2 1.965(4) . ?
Pd N2 1.965(4) 10_665 ?
Pd N1 1.973(3) . ?
Pd N1 1.973(3) 10_665 ?
O1 N1 1.342(4) . ?
O2 N2 1.391(4) . ?
N1 C1 1.305(5) . ?
N2 C2 1.296(5) . ?
N3 C1 1.369(5) . ?
N3 C11 1.431(7) . ?
N4 C2 1.348(5) . ?
N4 C21 1.460(7) . ?
C1 C2 1.485(6) . ?
C11 C12 1.521(9) . ?
C12 C13 1.429(11) . ?
C13 C14 1.535(15) . ?
C14 C15 1.36(2) . ?
C15 C16 1.21(2) . ?
C21 C22 1.219(11) . ?
C22 C23 1.385(11) . ?
C23 C24 1.483(12) . ?
C24 C25 1.448(14) . ?
C25 C26 1.408(14) . ?
