#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/90/2209021.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2209021
loop_
_publ_author_name
'Lindoy, Leonard F.'
'McMurtrie, John C.'
'Schilter, David'
_publ_section_title
'[4-(Dimethylamino)pyridine-κN]bis(pentane-2,4-dionato-κ²O,O')copper(II)'
_journal_coeditor_code           TK2030
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1142
_journal_page_last               m1143
_journal_paper_doi               10.1107/S1600536806014528
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Cu (C5 H7 O2)2 (C7 H10 N2)]'
_chemical_formula_moiety         'C17 H24 Cu N2 O4'
_chemical_formula_sum            'C17 H24 Cu N2 O4'
_chemical_formula_weight         383.92
_chemical_name_systematic
;
[4-(Dimethylamino)pyridine-\kN]bis(pentane-2,4-dionato-κ²O,O')copper(II)
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.3708(11)
_cell_length_b                   27.215(3)
_cell_length_c                   11.3000(11)
_cell_measurement_reflns_used    6762
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.7
_cell_volume                     3496.9(6)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT and XPREP (Siemens, 1995)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and WinGX32 (Farrugia, 1999)'
_computing_publication_material  'enCIFer (Allen et al.,  2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al.,  1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_av_sigmaI/netI    0.031
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8108
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         28.3
_diffrn_reflns_theta_min         2.7
_diffrn_standards_decay_%        0.20
_diffrn_standards_number         163
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_T_max  0.718
_exptl_absorpt_correction_T_min  0.633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.91
_refine_diff_density_min         -0.24
_refine_ls_abs_structure_details 'Flack (1983), 968 Friedel pairs'
_refine_ls_abs_structure_Flack   0.042(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2107
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.027
_refine_ls_R_factor_gt           0.026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0425P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.063
_refine_ls_wR_factor_ref         0.064
_reflns_number_gt                2048
_reflns_number_total             2107
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            tk2030.cif
_cod_data_source_block           I
_cod_database_code               2209021
_cod_database_fobs_code          2209021
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+1/4, -y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+1/4, -y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+3/4, -y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
C C1 0.92501(16) 0.36633(6) 1.07938(18) 0.0282(4) Uani d . 1
H H1A 0.9706 0.3856 1.0223 0.042 Uiso calc R 1
H H1B 0.9772 0.3432 1.1201 0.042 Uiso calc R 1
H H1C 0.8889 0.3884 1.1375 0.042 Uiso calc R 1
C C2 0.82995(15) 0.33823(6) 1.01499(15) 0.0216(3) Uani d . 1
C C3 0.71763(17) 0.35940(6) 1.00660(15) 0.0226(3) Uani d . 1
H H3 0.7049 0.3899 1.0454 0.027 Uiso calc R 1
C C4 0.62307(13) 0.33858(6) 0.94479(14) 0.0192(3) Uani d . 1
C C5 0.50990(15) 0.36720(8) 0.93475(18) 0.0266(4) Uani d . 1
H H5A 0.4442 0.3467 0.9614 0.040 Uiso calc R 1
H H5B 0.4973 0.3768 0.8521 0.040 Uiso calc R 1
H H5C 0.5147 0.3967 0.9842 0.040 Uiso calc R 1
C C6 0.65032(16) 0.25476(6) 0.64031(17) 0.0211(3) Uani d . 1
H H6 0.5786 0.2586 0.6825 0.025 Uiso calc R 1
C C7 0.6458(2) 0.25440(6) 0.5187(2) 0.0205(4) Uani d . 1
H H7 0.5722 0.2571 0.4795 0.025 Uiso calc R 1
C C8 0.7500 0.2500 0.4522(3) 0.0195(7) Uani d S 1
C C9 0.6391(3) 0.25096(6) 0.2669(2) 0.0254(5) Uani d . 1
H H9A 0.5992 0.2823 0.2810 0.038 Uiso calc R 1
H H9B 0.5888 0.2239 0.2939 0.038 Uiso calc R 1
H H9C 0.6546 0.2472 0.1820 0.038 Uiso calc R 1
N N1 0.7500 0.2500 0.7030(2) 0.0193(4) Uani d S 1
N N2 0.7500 0.2500 0.3317(3) 0.0238(7) Uani d S 1
O O1 0.86018(10) 0.29770(4) 0.97011(12) 0.0238(3) Uani d . 1
O O2 0.62307(9) 0.29708(4) 0.89236(13) 0.0216(2) Uani d . 1
Cu Cu1 0.7500 0.2500 0.89056(2) 0.01788(9) Uani d S 1
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'
Cu Cu 0.3201 1.2651 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
O1 C2 C3 . . 125.40(15) ?
O1 C2 C1 . . 116.18(15) ?
C3 C2 C1 . . 118.39(15) ?
C4 C3 C2 . . 124.43(16) ?
C4 C3 H3 . . 117.8 ?
C2 C3 H3 . . 117.8 ?
O2 C4 C3 . . 126.12(15) ?
O2 C4 C5 . . 114.98(14) ?
C3 C4 C5 . . 118.88(16) ?
C4 C5 H5A . . 109.5 ?
C4 C5 H5B . . 109.5 ?
H5A C5 H5B . . 109.5 ?
C4 C5 H5C . . 109.5 ?
H5A C5 H5C . . 109.5 ?
H5B C5 H5C . . 109.5 ?
N1 C6 C7 . . 123.93(19) ?
N1 C6 H6 . . 118.0 ?
C7 C6 H6 . . 118.0 ?
C6 C7 C8 . . 120.2(2) ?
C6 C7 H7 . . 119.9 ?
C8 C7 H7 . . 119.9 ?
N2 C8 C7 . 14_655 122.27(18) ?
N2 C8 C7 . . 122.27(18) ?
C7 C8 C7 14_655 . 115.5(4) ?
N2 C9 H9A . . 109.5 ?
N2 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
N2 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
C6 N1 C6 . 14_655 116.3(2) ?
C6 N1 Cu1 . . 121.86(11) ?
C6 N1 Cu1 14_655 . 121.86(11) ?
C8 N2 C9 . . 120.16(17) ?
C8 N2 C9 . 14_655 120.16(17) ?
C9 N2 C9 . 14_655 119.7(3) ?
C2 O1 Cu1 . . 124.96(11) ?
C4 O2 Cu1 . . 126.36(10) ?
O2 Cu1 O1 . 14_655 87.60(5) n
O2 Cu1 O1 14_655 14_655 91.86(5) n
O1 Cu1 O1 . 14_655 127.03(8) ?
O2 Cu1 N1 14_655 . 90.60(5) n
O1 Cu1 N1 14_655 . 116.48(4) n
O1 Cu1 O2 . . 91.86(5) y
O1 Cu1 N1 . . 116.48(4) y
O1 Cu1 O2 14_655 . 87.60(5) y
O2 Cu1 N1 . . 90.60(5) y
O2 Cu1 O2 . 14_655 178.79(9) y
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
C1 C2 . 1.511(2) ?
C1 H1A . 0.9800 ?
C1 H1B . 0.9800 ?
C1 H1C . 0.9800 ?
C2 O1 . 1.262(2) ?
C2 C3 . 1.404(2) ?
C3 C4 . 1.402(2) ?
C3 H3 . 0.9500 ?
C4 O2 . 1.275(2) ?
C4 C5 . 1.508(2) ?
C5 H5A . 0.9800 ?
C5 H5B . 0.9800 ?
C5 H5C . 0.9800 ?
C6 N1 . 1.343(2) ?
C6 C7 . 1.375(3) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.408(3) ?
C7 H7 . 0.9500 ?
C8 N2 . 1.361(3) ?
C9 N2 . 1.459(3) ?
C9 H9A . 0.9800 ?
C9 H9B . 0.9800 ?
C9 H9C . 0.9800 ?
N1 C6 14_655 1.343(2) ?
N2 C9 14_655 1.459(3) ?
Cu1 O1 14_655 2.0156(12) n
Cu1 O2 14_655 1.9301(10) n
Cu1 O1 . 2.0156(12) y
Cu1 O2 . 1.9301(10) y
Cu1 N1 . 2.119(2) y
C8 C7 14_655 1.408(3) ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
O1 C2 C3 C4 . . -1.1(3)
C1 C2 C3 C4 . . 176.81(16)
C2 C3 C4 O2 . . 3.3(3)
C2 C3 C4 C5 . . -175.16(17)
N1 C6 C7 C8 . . -1.5(3)
C6 C7 C8 N2 . . -179.28(12)
C6 C7 C8 C7 . 14_655 0.72(12)
C7 C6 N1 C6 . 14_655 0.78(13)
C7 C6 N1 Cu1 . . -179.22(13)
C7 C8 N2 C9 14_655 . 175.41(11)
C7 C8 N2 C9 . . -4.59(11)
C7 C8 N2 C9 14_655 14_655 -4.59(11)
C7 C8 N2 C9 . 14_655 175.41(11)
C3 C2 O1 Cu1 . . -7.0(2)
C1 C2 O1 Cu1 . . 174.97(11)
C3 C4 O2 Cu1 . . 3.5(2)
C5 C4 O2 Cu1 . . -177.97(13)
C4 O2 Cu1 O1 . . -8.17(14)
C4 O2 Cu1 O1 . 14_655 118.83(14)
C4 O2 Cu1 N1 . . -124.69(13)
C2 O1 Cu1 O2 . . 9.92(15)
C2 O1 Cu1 O2 . 14_655 -169.00(14)
C2 O1 Cu1 O1 . 14_655 -78.48(14)
C2 O1 Cu1 N1 . . 101.52(14)
C6 N1 Cu1 O2 . . -35.08(9)
C6 N1 Cu1 O2 14_655 . 144.92(9)
C6 N1 Cu1 O2 . 14_655 144.92(9)
C6 N1 Cu1 O2 14_655 14_655 -35.08(9)
C6 N1 Cu1 O1 . . -127.46(8)
C6 N1 Cu1 O1 14_655 . 52.54(8)
C6 N1 Cu1 O1 . 14_655 52.54(8)
C6 N1 Cu1 O1 14_655 14_655 -127.46(8)
