#------------------------------------------------------------------------------
#$Date: 2019-06-20 09:32:08 +0300 (Thu, 20 Jun 2019) $
#$Revision: 216139 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/15/1551529.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_1551529
loop_
_publ_author_name
'KASSIM, Karimah'
'KAHAR, Muhammad Ashraf Mohd'
'YAMIN, Bohari M.'
'MANAN, Mohd Abdul Fatah Abdul'
'YUSOF, M. Sukeri M.'
_publ_section_title
;
 Crystal Structure of
 Bis(2-methoxy-6-((Z)-(p-tolylimino)methyl)phenoxy)palladium
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              25
_journal_paper_doi               10.2116/xraystruct.35.25
_journal_volume                  35
_journal_year                    2019
_chemical_formula_moiety         'C30 H28 N2 O4 Pd'
_chemical_formula_sum            'C30 H28 N2 O4 Pd'
_chemical_formula_weight         586.94
_chemical_melting_point          560
_chemical_name_common
;
bis(2-methoxy-6-((Z)-(p-tolyimino)-
methyl)phenoxy)palladium
;
_chemical_name_systematic
;
bis(2-methoxy-6-((Z)-(p-tolyimino)-
methyl)phenoxy)palladium
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 97.327(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0221(14)
_cell_length_b                   11.6615(13)
_cell_length_c                   8.4898(9)
_cell_measurement_reflns_used    17828
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      2.9
_cell_volume                     1278.7(2)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'SMART (Bruker, 2009)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL- (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            24990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.365
_diffrn_reflns_theta_min         2.984
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (BRUKER, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.590
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         3186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0158P)²+2.4144P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2587
_reflns_number_total             3186
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            35_25_1.txt
_cod_data_source_block           b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 5642 2017-10-24 12:04:52Z antanas 
;
_cod_database_code               1551529
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.657
_shelx_estimated_absorpt_t_max   0.887
_shelxl_version_number           2013-3
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd1 Pd 0.0000 0.0000 0.0000 0.02505(9) Uani 1 2 d S . P
O1 O 0.33445(17) 0.0456(2) 0.1951(3) 0.0511(6) Uani 1 1 d . . .
O2 O 0.15057(15) 0.01459(19) 0.0543(3) 0.0384(5) Uani 1 1 d . . .
N1 N -0.01956(17) 0.09270(19) 0.1951(3) 0.0282(5) Uani 1 1 d . . .
C1 C 0.1992(2) -0.1427(2) -0.1031(3) 0.0312(6) Uani 1 1 d . . .
C2 C 0.2801(3) -0.2164(3) -0.1352(4) 0.0471(8) Uani 1 1 d . . .
H2A H 0.2672 -0.2728 -0.2126 0.056 Uiso 1 1 calc R U .
C3 C 0.3773(3) -0.2058(3) -0.0537(5) 0.0548(9) Uani 1 1 d . . .
H3A H 0.4293 -0.2566 -0.0728 0.066 Uiso 1 1 calc R U .
C4 C 0.3981(2) -0.1186(3) 0.0581(4) 0.0449(8) Uani 1 1 d . . .
H4A H 0.4648 -0.1104 0.1108 0.054 Uiso 1 1 calc R U .
C5 C 0.3222(2) -0.0449(3) 0.0914(3) 0.0339(6) Uani 1 1 d . . .
C6 C 0.2189(2) -0.0563(2) 0.0133(3) 0.0287(5) Uani 1 1 d . . .
C7 C 0.4276(3) 0.0541(4) 0.2962(5) 0.0603(10) Uani 1 1 d . . .
H7A H 0.4261 0.1209 0.3618 0.090 Uiso 1 1 calc R U .
H7B H 0.4841 0.0600 0.2341 0.090 Uiso 1 1 calc R U .
H7C H 0.4367 -0.0130 0.3621 0.090 Uiso 1 1 calc R U .
C8 C -0.1034(2) 0.1492(2) 0.2080(3) 0.0319(6) Uani 1 1 d . . .
C9 C 0.0636(2) 0.1016(2) 0.3237(3) 0.0292(5) Uani 1 1 d . . .
C10 C 0.1113(2) 0.0024(2) 0.3844(3) 0.0331(6) Uani 1 1 d . . .
H10A H 0.0896 -0.0684 0.3420 0.040 Uiso 1 1 calc R U .
C11 C 0.1913(2) 0.0081(3) 0.5083(3) 0.0373(6) Uani 1 1 d . . .
H11A H 0.2234 -0.0590 0.5478 0.045 Uiso 1 1 calc R U .
C12 C 0.2242(2) 0.1129(3) 0.5740(3) 0.0379(7) Uani 1 1 d . . .
C13 C 0.1759(2) 0.2114(3) 0.5127(4) 0.0389(7) Uani 1 1 d . . .
H13A H 0.1968 0.2821 0.5560 0.047 Uiso 1 1 calc R U .
C14 C 0.0963(2) 0.2065(3) 0.3871(3) 0.0358(6) Uani 1 1 d . . .
H14A H 0.0652 0.2736 0.3458 0.043 Uiso 1 1 calc R U .
C15 C 0.3124(3) 0.1203(4) 0.7074(4) 0.0551(9) Uani 1 1 d . . .
H15A H 0.3241 0.1990 0.7373 0.083 Uiso 1 1 calc R U .
H15B H 0.3740 0.0891 0.6727 0.083 Uiso 1 1 calc R U .
H15C H 0.2953 0.0774 0.7970 0.083 Uiso 1 1 calc R U .
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
O2 Pd1 O2 180.0 3 .
O2 Pd1 N1 90.71(8) 3 .
O2 Pd1 N1 89.29(8) . .
O2 Pd1 N1 89.29(8) 3 3
O2 Pd1 N1 90.71(8) . 3
N1 Pd1 N1 180.00(7) . 3
C5 O1 C7 118.0(3) . .
C6 O2 Pd1 125.55(18) . .
C8 N1 C9 117.5(2) . .
C8 N1 Pd1 122.59(19) . .
C9 N1 Pd1 119.90(17) . .
C6 C1 C2 119.7(3) . .
C6 C1 C8 122.4(2) . 3
C2 C1 C8 117.2(3) . 3
C3 C2 C1 120.8(3) . .
C3 C2 H2A 119.6 . .
C1 C2 H2A 119.6 . .
C2 C3 C4 119.9(3) . .
C2 C3 H3A 120.1 . .
C4 C3 H3A 120.1 . .
C5 C4 C3 121.1(3) . .
C5 C4 H4A 119.4 . .
C3 C4 H4A 119.4 . .
C4 C5 O1 126.2(3) . .
C4 C5 C6 120.6(3) . .
O1 C5 C6 113.3(2) . .
O2 C6 C1 125.1(2) . .
O2 C6 C5 117.0(2) . .
C1 C6 C5 117.9(2) . .
O1 C7 H7A 109.5 . .
O1 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
O1 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N1 C8 C1 126.6(3) . 3
C10 C9 C14 119.6(2) . .
C10 C9 N1 118.8(2) . .
C14 C9 N1 121.6(2) . .
C9 C10 C11 120.2(3) . .
C9 C10 H10A 119.9 . .
C11 C10 H10A 119.9 . .
C10 C11 C12 120.8(3) . .
C10 C11 H11A 119.6 . .
C12 C11 H11A 119.6 . .
C13 C12 C11 118.6(3) . .
C13 C12 C15 120.2(3) . .
C11 C12 C15 121.2(3) . .
C12 C13 C14 121.0(3) . .
C12 C13 H13A 119.5 . .
C14 C13 H13A 119.5 . .
C9 C14 C13 119.9(3) . .
C9 C14 H14A 120.1 . .
C13 C14 H14A 120.1 . .
C12 C15 H15A 109.5 . .
C12 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C12 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 O2 1.9636(19) 3
Pd1 O2 1.9636(19) .
Pd1 N1 2.021(2) .
Pd1 N1 2.021(2) 3
O1 C5 1.371(4) .
O1 C7 1.398(4) .
O2 C6 1.295(3) .
N1 C8 1.292(3) .
N1 C9 1.440(3) .
C1 C6 1.412(4) .
C1 C2 1.413(4) .
C1 C8 1.439(4) 3
C2 C3 1.368(5) .
C2 H2A 0.9300 .
C3 C4 1.393(5) .
C3 H3A 0.9300 .
C4 C5 1.366(4) .
C4 H4A 0.9300 .
C5 C6 1.428(4) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 C1 1.439(4) 3
C9 C10 1.381(4) .
C9 C14 1.382(4) .
C10 C11 1.384(4) .
C10 H10A 0.9300 .
C11 C12 1.388(4) .
C11 H11A 0.9300 .
C12 C13 1.380(4) .
C12 C15 1.509(4) .
C13 C14 1.389(4) .
C13 H13A 0.9300 .
C14 H14A 0.9300 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
