#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2007363.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_2007363
loop_
_publ_author_name
'Yang, G.'
'Tong, M.-L.'
'Chen, X.-M.'
'Ng, S. W.'
_publ_section_title
;
Bis(di-2-pyridylmethanediol-N,O,N')copper(II)
Diperchlorate
;
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 732
_journal_page_last 734
_journal_volume 54
_journal_year 1998
_chemical_formula_iupac '[Cu (C11 H10 N2 O2)2] (Cl1 O4)2'
_chemical_formula_moiety 'C22 H20 Cu N4 O4 , 2(Cl O4)'
_chemical_formula_structural '[(C~11~H~10~N~2~O~2~)~2~Cu] 2[ClO~4~]'
_chemical_formula_sum 'C22 H20 Cl2 Cu N4 O12'
_chemical_formula_weight 666.86
_chemical_name_systematic
;
Bis(di-2-pyridylmethandiol)copper(II) diperchlorate
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_audit_creation_method SHELXL
_cell_angle_alpha 90.00
_cell_angle_beta 100.830(4)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 7.8466(3)
_cell_length_b 13.6602(4)
_cell_length_c 12.2522(5)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 15.0
_cell_measurement_theta_min 12.0
_cell_volume 1289.88(8)
_computing_cell_refinement 'CAD-4 VAX/PC'
_computing_data_collection 'CAD-4 VAX/PC (Enraf-Nonius, 1988)'
_computing_data_reduction 'Xtal3.0 (Hall & Stewart, 1990)'
_computing_molecular_graphics 'ORTEPII (Johnson, 1976)'
_computing_publication_material SHELXL93
_computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution 'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature 298(2)
_diffrn_measurement_device 'Enraf-Nonius CAD-4'
_diffrn_measurement_method \w
_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 0.011
_diffrn_reflns_av_sigmaI/netI 0.019
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 3990
_diffrn_reflns_theta_max 29.96
_diffrn_reflns_theta_min 2.26
_diffrn_standards_decay_% none
_diffrn_standards_interval_time 60
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 1.127
_exptl_absorpt_correction_T_max 0.697
_exptl_absorpt_correction_T_min 0.613
_exptl_absorpt_correction_type '\y scan (North et al., 1968)'
_exptl_crystal_colour Lilac
_exptl_crystal_density_diffrn 1.717
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'Regular block'
_exptl_crystal_F_000 678
_exptl_crystal_size_max 0.44
_exptl_crystal_size_mid 0.36
_exptl_crystal_size_min 0.32
_refine_diff_density_max 0.54
_refine_diff_density_min -0.48
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_all 1.026
_refine_ls_goodness_of_fit_obs 1.057
_refine_ls_hydrogen_treatment 'H atoms: see below'
_refine_ls_matrix_type full
_refine_ls_number_parameters 195
_refine_ls_number_reflns 3746
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.026
_refine_ls_restrained_S_obs 1.057
_refine_ls_R_factor_all 0.057
_refine_ls_R_factor_obs 0.044
_refine_ls_shift/esd_max 0.001
_refine_ls_shift/esd_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0707P)^2^+0.9966P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all 0.131
_refine_ls_wR_factor_obs 0.120
_reflns_number_observed 3037
_reflns_number_total 3746
_reflns_observed_criterion I>2\s(I)
_[local]_cod_data_source_file na1335.cif
_[local]_cod_data_source_block cubpt
_[local]_cod_cif_authors_sg_H-M 'P 21/n'
_[local]_cod_chemical_formula_sum_orig 'C22 H20 N4 O12 Cl2 Cu'
_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 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_database_code 2007363
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cu1 0.0328(2) 0.0253(2) 0.0267(2) -0.00062(14) 0.00843(13) 0.00091(13)
Cl1 0.0773(5) 0.0569(4) 0.0366(3) 0.0015(4) 0.0139(3) 0.0125(3)
O1 0.0417(9) 0.0388(9) 0.0356(9) -0.0032(7) -0.0024(7) 0.0076(7)
O2 0.092(2) 0.0499(12) 0.0282(9) -0.0080(11) 0.0148(10) -0.0104(9)
O3 0.178(4) 0.235(5) 0.0347(14) 0.031(4) 0.033(2) 0.024(2)
O4 0.125(3) 0.123(3) 0.115(3) -0.020(2) 0.065(2) 0.019(2)
O5 0.093(3) 0.164(4) 0.125(3) 0.017(3) -0.008(2) 0.064(3)
O6 0.275(9) 0.051(2) 0.118(3) 0.024(3) -0.019(4) 0.009(2)
N1 0.0341(9) 0.0290(8) 0.0315(9) -0.0019(7) 0.0073(7) 0.0020(7)
N2 0.0361(9) 0.0285(9) 0.0279(8) 0.0011(7) 0.0064(7) 0.0030(7)
C1 0.0379(12) 0.0323(11) 0.0475(13) -0.0042(9) 0.0050(10) 0.0008(10)
C2 0.0376(13) 0.0477(15) 0.061(2) -0.0083(11) 0.0059(12) 0.0136(13)
C3 0.0389(13) 0.072(2) 0.056(2) -0.0014(13) 0.0191(12) 0.0185(15)
C4 0.0464(14) 0.060(2) 0.0384(13) 0.0063(12) 0.0183(11) 0.0043(11)
C5 0.0380(11) 0.0340(10) 0.0285(10) 0.0017(9) 0.0088(8) 0.0035(8)
C6 0.0443(13) 0.0395(12) 0.0332(11) 0.0022(10) 0.0086(9) 0.0089(9)
C7 0.052(2) 0.0399(14) 0.054(2) 0.0040(11) 0.0072(12) 0.0190(12)
C8 0.064(2) 0.0299(12) 0.067(2) 0.0096(12) 0.0111(15) 0.0065(12)
C9 0.059(2) 0.0325(12) 0.0485(14) 0.0047(11) 0.0102(12) -0.0072(10)
C10 0.0384(11) 0.0293(10) 0.0303(10) -0.0017(8) 0.0045(8) -0.0012(8)
C11 0.0468(13) 0.0360(11) 0.0244(9) -0.0017(10) 0.0062(9) -0.0016(8)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Cu1 0 0 0 0.02790(10) Uani d S 1 Cu
Cl1 0.15520(10) -0.11694(6) -0.59045(6) 0.0565(2) Uani d . 1 Cl
O1 -0.0804(2) -0.06710(10) -0.1884(2) 0.0400(4) Uani d . 1 O
O2 0.0967(4) -0.1636(2) -0.2783(2) 0.0562(6) Uani d . 1 O
O3 0.1849(6) -0.1100(4) -0.4768(2) 0.148(2) Uani d . 1 O
O4 0.2718(5) -0.0564(3) -0.6342(3) 0.1160(10) Uani d . 1 O
O5 -0.0048(5) -0.0782(3) -0.6431(4) 0.131(2) Uani d . 1 O
O6 0.1780(10) -0.2116(3) -0.6234(4) 0.190(3) Uani d . 1 O
N1 0.2032(3) 0.02810(10) -0.0734(2) 0.0314(4) Uani d . 1 N
N2 0.0700(3) -0.14180(10) 0.0066(2) 0.0308(4) Uani d . 1 N
C1 0.3168(3) 0.1007(2) -0.0414(2) 0.0396(5) Uani d . 1 C
H1 0.3015(3) 0.1409(2) 0.0173(2) 0.059 Uiso calc R 1 H
C2 0.4558(4) 0.1172(2) -0.0934(3) 0.0492(7) Uani d . 1 C
H2 0.5327(4) 0.1683(2) -0.0707(3) 0.074 Uiso calc R 1 H
C3 0.4783(4) 0.0567(3) -0.1792(3) 0.0544(8) Uani d . 1 C
H3 0.5708(4) 0.0669(3) -0.2156(3) 0.082 Uiso calc R 1 H
C4 0.3630(4) -0.0194(2) -0.2115(2) 0.0468(6) Uani d . 1 C
H4 0.3784(4) -0.0618(2) -0.2682(2) 0.070 Uiso calc R 1 H
C5 0.2248(3) -0.0307(2) -0.1578(2) 0.0332(4) Uani d . 1 C
C6 0.0868(3) -0.1980(2) 0.0979(2) 0.0388(5) Uani d . 1 C
H6 0.0583(3) -0.1718(2) 0.1622(2) 0.058 Uiso calc R 1 H
C7 0.1446(4) -0.2928(2) 0.0992(3) 0.0489(6) Uani d . 1 C
H7 0.1557(4) -0.3303(2) 0.1636(3) 0.073 Uiso calc R 1 H
C8 0.1862(4) -0.3319(2) 0.0035(3) 0.0539(7) Uani d . 1 C
H8 0.2263(4) -0.3959(2) 0.0029(3) 0.081 Uiso calc R 1 H
C9 0.1676(4) -0.2751(2) -0.0910(2) 0.0467(6) Uani d . 1 C
H9 0.1948(4) -0.2999(2) -0.1563(2) 0.070 Uiso calc R 1 H
C10 0.1075(3) -0.1803(2) -0.0865(2) 0.0329(4) Uani d . 1 C
C11 0.0860(3) -0.1102(2) -0.1843(2) 0.0358(5) Uani d . 1 C
H11 -0.099(5) -0.034(3) -0.235(3) 0.060(10) Uiso d . 1 H
H21 0.104(5) -0.135(3) -0.324(3) 0.060(10) Uiso d . 1 H
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'
Cl Cl 0.1484 0.1585 '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
N1 Cu1 N1 . 3 180 ?
N1 Cu1 N2 . 3 91.80(10) yes
N1 Cu1 N2 3 3 88.20(10) ?
N1 Cu1 N2 . . 88.20(10) yes
N1 Cu1 N2 3 . 91.80(10) ?
N2 Cu1 N2 3 . 180.0 ?
N1 Cu1 O1 . . 74.70(10) yes
N1 Cu1 O1 3 . 105.40(10) ?
N2 Cu1 O1 3 . 107.60(10) ?
N2 Cu1 O1 . . 72.40(10) yes
O3 Cl1 O6 . . 110.9(3) ?
O3 Cl1 O5 . . 114.0(3) ?
O6 Cl1 O5 . . 112.0(4) ?
O3 Cl1 O4 . . 110.3(3) ?
O6 Cl1 O4 . . 108.1(4) ?
O5 Cl1 O4 . . 101.1(3) ?
C11 O1 Cu1 . . 92.80(10) yes
C1 N1 C5 . . 119.6(2) ?
C1 N1 Cu1 . . 123.3(2) yes
C5 N1 Cu1 . . 117.1(2) yes
C10 N2 C6 . . 118.8(2) ?
C10 N2 Cu1 . . 116.6(2) yes
C6 N2 Cu1 . . 124.6(2) yes
N1 C1 C2 . . 121.6(3) ?
C3 C2 C1 . . 118.8(3) ?
C2 C3 C4 . . 119.8(3) ?
C5 C4 C3 . . 118.6(3) ?
N1 C5 C4 . . 121.6(2) ?
N1 C5 C11 . . 113.6(2) ?
C4 C5 C11 . . 124.8(2) ?
N2 C6 C7 . . 122.0(2) ?
C6 C7 C8 . . 119.0(3) ?
C9 C8 C7 . . 119.4(3) ?
C8 C9 C10 . . 118.5(3) ?
N2 C10 C9 . . 122.3(2) ?
N2 C10 C11 . . 114.5(2) ?
C9 C10 C11 . . 123.2(2) ?
O2 C11 O1 . . 112.8(2) ?
O2 C11 C10 . . 108.1(2) ?
O1 C11 C10 . . 104.7(2) ?
O2 C11 C5 . . 113.6(2) ?
O1 C11 C5 . . 109.0(2) ?
C10 C11 C5 . . 108.1(2) ?
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
Cu1 N1 . 2.009(2) yes
Cu1 N1 3 2.009(2) ?
Cu1 N2 3 2.010(2) ?
Cu1 N2 . 2.010(2) yes
Cu1 O1 . 2.454(2) yes
Cl1 O3 . 1.371(3) ?
Cl1 O6 . 1.377(4) ?
Cl1 O5 . 1.404(4) ?
Cl1 O4 . 1.411(3) ?
O1 C11 . 1.425(3) yes
O2 C11 . 1.379(3) yes
N1 C1 . 1.342(3) ?
N1 C5 . 1.344(3) ?
N2 C10 . 1.338(3) ?
N2 C6 . 1.343(3) ?
C1 C2 . 1.381(4) ?
C2 C3 . 1.375(5) ?
C3 C4 . 1.386(5) ?
C4 C5 . 1.379(3) ?
C5 C11 . 1.529(3) ?
C6 C7 . 1.372(4) ?
C7 C8 . 1.382(5) ?
C8 C9 . 1.379(4) ?
C9 C10 . 1.382(3) ?
C10 C11 . 1.518(3) ?