#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/43/7024310.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_7024310
loop_
_publ_author_name
'Bailey, Philip J.'
'Collins, Anna'
'Haack, Peter'
'Parsons, Simon'
'Rahman, Mahmudur'
'Smith, Damian'
'White, Fraser J.'
_publ_section_related_literature
;
?
;
_publ_section_title
;
 Palladium complexes of 6-aminofulvene-2-aldiminate (AFA) ligands.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1591
_journal_page_last               1597
_journal_paper_doi               10.1039/b914707a
_journal_volume                  39
_journal_year                    2010
_chemical_compound_source        'Mohammed Mahmudun Rahman, MMR163'
_chemical_formula_moiety         'C38 H54 N4 Pd1'
_chemical_formula_sum            'C38 H54 N4 Pd'
_chemical_formula_weight         673.27
_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
_audit_creation_date             07-10-26
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 101.6900(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4867(2)
_cell_length_b                   16.9336(3)
_cell_length_c                   10.6112(2)
_cell_measurement_reflns_used    8119
_cell_measurement_temperature    150
_cell_measurement_theta_max      31
_cell_measurement_theta_min      2
_cell_volume                     1669.27(6)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       'Bruker SMART'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21684
_diffrn_reflns_theta_full        28.655
_diffrn_reflns_theta_max         30.484
_diffrn_reflns_theta_min         2.192
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_recrystallization_method
;
Slow evaporation of toluene and acetonitrile in ice bath under N₂.
;
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.61
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8712
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         4918
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.000250
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[σ²(F²) + ( 0.01P)² + 0.00P]
,where P=(max(Fo²,0) + 2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0794
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0794
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                3757
_reflns_number_total             4918
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0517
_oxford_refine_ls_scale          0.4506(4)
_oxford_reflns_number_all        4918
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            b914707a.txt
_cod_data_source_block           PB7002
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C38 H54 N4 Pd1'
_cod_database_code               7024310
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
Pd1 Pd 0.0000 0.5000 0.5000 0.0146 1.0000 Uani S
N2 N 0.0397(2) 0.54170(11) 0.33058(17) 0.0172 1.0000 Uani .
C3 C 0.1714(2) 0.51269(12) 0.2897(2) 0.0186 1.0000 Uani .
C4 C 0.1648(3) 0.51182(15) 0.1445(2) 0.0271 1.0000 Uani .
C5 C 0.3050(3) 0.47997(15) 0.1155(2) 0.0296 1.0000 Uani .
C6 C 0.4309(3) 0.53040(16) 0.1801(3) 0.0330 1.0000 Uani .
C7 C 0.4412(3) 0.53153(18) 0.3251(3) 0.0344 1.0000 Uani .
C8 C 0.3004(3) 0.56062(16) 0.3584(3) 0.0307 1.0000 Uani .
C9 C -0.0544(2) 0.58355(13) 0.2523(2) 0.0199 1.0000 Uani .
C10 C -0.1723(2) 0.62732(12) 0.2783(2) 0.0186 1.0000 Uani .
C11 C -0.1964(2) 0.66123(13) 0.3969(2) 0.0189 1.0000 Uani .
C12 C -0.1105(2) 0.66069(13) 0.5229(2) 0.0191 1.0000 Uani .
N13 N -0.01049(19) 0.61119(10) 0.57375(17) 0.0164 1.0000 Uani .
C14 C 0.0804(2) 0.62859(13) 0.7026(2) 0.0178 1.0000 Uani .
C15 C 0.2380(2) 0.62143(14) 0.6950(2) 0.0232 1.0000 Uani .
C16 C 0.3365(3) 0.63442(15) 0.8269(2) 0.0286 1.0000 Uani .
C17 C 0.3073(3) 0.71246(16) 0.8854(3) 0.0338 1.0000 Uani .
C18 C 0.1495(3) 0.72005(16) 0.8921(2) 0.0299 1.0000 Uani .
C19 C 0.0508(3) 0.70803(14) 0.7608(2) 0.0232 1.0000 Uani .
C20 C -0.3119(3) 0.71497(14) 0.3625(2) 0.0239 1.0000 Uani .
C21 C -0.3607(3) 0.71401(14) 0.2295(2) 0.0264 1.0000 Uani .
C22 C -0.2747(3) 0.66204(14) 0.1774(2) 0.0233 1.0000 Uani .
H31 H 0.1868 0.4573 0.3180 0.0207 1.0000 Uiso R
H42 H 0.1514 0.5654 0.1109 0.0328 1.0000 Uiso R
H41 H 0.0858 0.4776 0.1030 0.0328 1.0000 Uiso R
H51 H 0.2975 0.4776 0.0249 0.0357 1.0000 Uiso R
H52 H 0.3180 0.4263 0.1502 0.0358 1.0000 Uiso R
H62 H 0.4170 0.5843 0.1508 0.0396 1.0000 Uiso R
H61 H 0.5213 0.5097 0.1640 0.0391 1.0000 Uiso R
H72 H 0.5205 0.5658 0.3614 0.0409 1.0000 Uiso R
H71 H 0.4578 0.4778 0.3577 0.0415 1.0000 Uiso R
H81 H 0.2841 0.6143 0.3262 0.0373 1.0000 Uiso R
H82 H 0.3034 0.5555 0.4503 0.0370 1.0000 Uiso R
H91 H -0.0443 0.5861 0.1680 0.0236 1.0000 Uiso R
H121 H -0.1320 0.7025 0.5755 0.0220 1.0000 Uiso R
H141 H 0.0592 0.5881 0.7627 0.0197 1.0000 Uiso R
H152 H 0.2612 0.6599 0.6349 0.0272 1.0000 Uiso R
H151 H 0.2545 0.5685 0.6649 0.0273 1.0000 Uiso R
H161 H 0.4359 0.6328 0.8157 0.0297 1.0000 Uiso R
H162 H 0.3234 0.5917 0.8852 0.0302 1.0000 Uiso R
H172 H 0.3665 0.7154 0.9707 0.0358 1.0000 Uiso R
H171 H 0.3354 0.7556 0.8333 0.0366 1.0000 Uiso R
H182 H 0.1297 0.7726 0.9217 0.0322 1.0000 Uiso R
H181 H 0.1253 0.6799 0.9510 0.0319 1.0000 Uiso R
H191 H 0.0659 0.7503 0.7037 0.0266 1.0000 Uiso R
H192 H -0.0499 0.7100 0.7697 0.0270 1.0000 Uiso R
H201 H -0.3474 0.7463 0.4210 0.0259 1.0000 Uiso R
H211 H -0.4361 0.7435 0.1849 0.0295 1.0000 Uiso R
H221 H -0.2799 0.6507 0.0900 0.0256 1.0000 Uiso R
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N13 2_566 Pd1 N2 2_566 92.90(7) yes
N13 2_566 Pd1 N2 . 87.10(7) yes
N2 2_566 Pd1 N2 . 179.994 yes
N13 2_566 Pd1 N13 . 179.994 yes
N2 2_566 Pd1 N13 . 87.10(7) yes
N2 . Pd1 N13 . 92.90(7) yes
Pd1 . N2 C3 . 117.38(13) yes
Pd1 . N2 C9 . 121.82(15) yes
C3 . N2 C9 . 120.19(18) yes
N2 . C3 C4 . 115.58(18) yes
N2 . C3 C8 . 108.97(18) yes
C4 . C3 C8 . 110.61(19) yes
N2 . C3 H31 . 107.8 no
C4 . C3 H31 . 105.7 no
C8 . C3 H31 . 107.8 no
C3 . C4 C5 . 110.3(2) yes
C3 . C4 H42 . 109.6 no
C5 . C4 H42 . 108.1 no
C3 . C4 H41 . 109.3 no
C5 . C4 H41 . 108.6 no
H42 . C4 H41 . 110.9 no
C4 . C5 C6 . 110.5(2) yes
C4 . C5 H51 . 109.2 no
C6 . C5 H51 . 111.9 no
C4 . C5 H52 . 107.5 no
C6 . C5 H52 . 109.0 no
H51 . C5 H52 . 108.6 no
C5 . C6 C7 . 110.4(2) yes
C5 . C6 H62 . 110.1 no
C7 . C6 H62 . 106.9 no
C5 . C6 H61 . 111.1 no
C7 . C6 H61 . 107.7 no
H62 . C6 H61 . 110.6 no
C6 . C7 C8 . 110.9(2) yes
C6 . C7 H72 . 107.2 no
C8 . C7 H72 . 111.1 no
C6 . C7 H71 . 108.6 no
C8 . C7 H71 . 107.8 no
H72 . C7 H71 . 111.2 no
C7 . C8 C3 . 111.8(2) yes
C7 . C8 H81 . 107.7 no
C3 . C8 H81 . 106.0 no
C7 . C8 H82 . 110.6 no
C3 . C8 H82 . 106.8 no
H81 . C8 H82 . 113.9 no
N2 . C9 C10 . 129.0(2) yes
N2 . C9 H91 . 117.0 no
C10 . C9 H91 . 114.0 no
C9 . C10 C11 . 130.5(2) yes
C9 . C10 C22 . 121.1(2) yes
C11 . C10 C22 . 106.7(2) yes
C10 . C11 C12 . 131.1(2) yes
C10 . C11 C20 . 106.44(19) yes
C12 . C11 C20 . 121.0(2) yes
C11 . C12 N13 . 128.9(2) yes
C11 . C12 H121 . 113.5 no
N13 . C12 H121 . 117.6 no
C12 . N13 Pd1 . 121.49(15) yes
C12 . N13 C14 . 119.46(18) yes
Pd1 . N13 C14 . 117.91(13) yes
N13 . C14 C15 . 109.22(17) yes
N13 . C14 C19 . 115.13(18) yes
C15 . C14 C19 . 110.78(19) yes
N13 . C14 H141 . 107.5 no
C15 . C14 H141 . 108.2 no
C19 . C14 H141 . 105.8 no
C14 . C15 C16 . 111.43(19) yes
C14 . C15 H152 . 109.8 no
C16 . C15 H152 . 109.1 no
C14 . C15 H151 . 108.5 no
C16 . C15 H151 . 108.8 no
H152 . C15 H151 . 109.2 no
C15 . C16 C17 . 111.8(2) yes
C15 . C16 H161 . 108.1 no
C17 . C16 H161 . 109.7 no
C15 . C16 H162 . 109.9 no
C17 . C16 H162 . 109.3 no
H161 . C16 H162 . 107.9 no
C16 . C17 C18 . 111.0(2) yes
C16 . C17 H172 . 108.1 no
C18 . C17 H172 . 110.0 no
C16 . C17 H171 . 109.0 no
C18 . C17 H171 . 110.2 no
H172 . C17 H171 . 108.4 no
C17 . C18 C19 . 111.9(2) yes
C17 . C18 H182 . 110.4 no
C19 . C18 H182 . 107.0 no
C17 . C18 H181 . 109.3 no
C19 . C18 H181 . 108.0 no
H182 . C18 H181 . 110.0 no
C14 . C19 C18 . 110.91(19) yes
C14 . C19 H191 . 109.6 no
C18 . C19 H191 . 109.4 no
C14 . C19 H192 . 109.3 no
C18 . C19 H192 . 109.7 no
H191 . C19 H192 . 107.9 no
C11 . C20 C21 . 109.6(2) yes
C11 . C20 H201 . 124.2 no
C21 . C20 H201 . 126.3 no
C20 . C21 C22 . 108.0(2) yes
C20 . C21 H211 . 125.3 no
C22 . C21 H211 . 126.7 no
C10 . C22 C21 . 109.2(2) yes
C10 . C22 H221 . 123.5 no
C21 . C22 H221 . 127.3 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 N13 2_566 2.0491(17) yes
Pd1 N2 2_566 2.0364(18) yes
Pd1 N2 . 2.0364(18) yes
Pd1 N13 . 2.0491(17) yes
N2 C3 . 1.487(3) yes
N2 C9 . 1.300(3) yes
C3 C4 . 1.529(3) yes
C3 C8 . 1.525(3) yes
C3 H31 . 0.988 no
C4 C5 . 1.524(3) yes
C4 H42 . 0.974 no
C4 H41 . 0.979 no
C5 C6 . 1.514(4) yes
C5 H51 . 0.950 no
C5 H52 . 0.979 no
C6 C7 . 1.522(4) yes
C6 H62 . 0.965 no
C6 H61 . 0.973 no
C7 C8 . 1.531(3) yes
C7 H72 . 0.967 no
C7 H71 . 0.974 no
C8 H81 . 0.972 no
C8 H82 . 0.974 no
C9 C10 . 1.415(3) yes
C9 H91 . 0.920 no
C10 C11 . 1.442(3) yes
C10 C22 . 1.419(3) yes
C11 C12 . 1.418(3) yes
C11 C20 . 1.414(3) yes
C12 N13 . 1.299(3) yes
C12 H121 . 0.950 no
N13 C14 . 1.490(3) yes
C14 C15 . 1.517(3) yes
C14 C19 . 1.530(3) yes
C14 H141 . 0.984 no
C15 C16 . 1.533(3) yes
C15 H152 . 0.968 no
C15 H151 . 0.975 no
C16 C17 . 1.509(3) yes
C16 H161 . 0.975 no
C16 H162 . 0.975 no
C17 C18 . 1.519(4) yes
C17 H172 . 0.965 no
C17 H171 . 0.985 no
C18 C19 . 1.527(3) yes
C18 H182 . 0.975 no
C18 H181 . 0.982 no
C19 H191 . 0.967 no
C19 H192 . 0.980 no
C20 C21 . 1.394(3) yes
C20 H201 . 0.929 no
C21 C22 . 1.389(3) yes
C21 H211 . 0.921 no
C22 H221 . 0.938 no
