#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/51/2015105.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_2015105
loop_
_publ_author_name
'Lea Glažar'
'Marjeta Radišek'
'Primož Šegedin'
'Amalija Golobič'
_publ_section_title
;Di-μ-formato-1κ²O:2κ²O'-di-μ-pyridin-2-olato-1κO:2κN;1κN:2κO-bis[(2-pyridone-κO)copper(II)]
 acetonitrile 1.02-solvate
;
_journal_coeditor_code           AV1269
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m526
_journal_page_last               m528
_journal_paper_doi               10.1107/S0108270105033871
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac
'[Cu2 (C H O2)2 (C5 H4 N O)2 (C5 H5 N O)2], 1.02(3)C H3 C N'
_chemical_formula_moiety         'C22 H20 Cu2 N4 O8, 1.02C2 H3 N'
_chemical_formula_sum            'C24.04 H23.06 Cu2 N5.02 O8'
_chemical_formula_weight         637.39
_chemical_name_systematic
;
Di-μ-formato-1κ²O:2κ²O'-di-μ-pyridin-2-olato-1\kO:2\kN;1\kN:2\kO-
bis[(2-pyridone-\kO)copper(II)] acetonitrile 1.02-solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 101.078(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.1571(8)
_cell_length_b                   15.3971(5)
_cell_length_c                   7.1673(2)
_cell_measurement_reflns_used    3136
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     2832.80(15)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'Xtal3.6 and PLATON (Spek, 2003)'
_computing_structure_refinement  'Xtal3.6 (Hall et al., 1999)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans with κ offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .026
_diffrn_reflns_av_sigmaI/netI    .038
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            13938
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.92
_exptl_absorpt_coefficient_mu    1.55
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       plate
_exptl_crystal_F_000             1297.8
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.388
_refine_diff_density_min         -1.155
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       0.000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.093
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_constraints    5
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2986
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .066
_refine_ls_R_factor_gt           .050
_refine_ls_shift/su_max          .001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;A Regina weighting scheme (Wang & Robertson, 1985) using the normal
equation
 of the second order was applied for individual reflections so that w=
A(0,0)
 + A(1,0)V(F) + A(0,1)V(S) + A(2,0)V(F)² + A(0,2)V(S)² +
A(1,1)V(F)V(S),
 where V(F)= Fobs/Fobs(max), Fobs(max)= 274.38
 and
V(S)=(sinθ/λ)/((sinθ/λ)(max)), (sinθ/λ)(max)= 0.6486. The
 parameters
were: A(0,0)=151.7662, A(1,0)=0.0099395, A(0,1)=-587.9600,
 A(2,0)=-0.0003962,
A(1,1)=0.0243166 , A(0,2)=570.2360.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .048
_refine_ls_wR_factor_ref         .044
_reflns_number_gt                2605
_reflns_number_total             3182
_reflns_threshold_expression     F²>2σ(F²)
_cod_data_source_file            av1269.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     -c_2yc
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2015105
_cod_database_fobs_code          2015105
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,+y,1/2-z
-x,-y,-z
+x,-y,1/2+z
1/2+x,1/2+y,+z
1/2-x,1/2+y,1/2-z
1/2-x,1/2-y,-z
1/2+x,1/2-y,1/2+z
loop_
_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_calc_attached_atom
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu .296520(10) .28380(2) .06522(5) .0226(2) Uani ? ? 1.00000 ? ?
O2 .37017(9) .34656(15) .1603(3) .0300(10) Uani ? ? 1.00000 ? ?
O4 .26485(9) .38256(14) -.0887(3) .0295(9) Uani ? ? 1.00000 ? ?
O11 .26384(9) .32483(15) .2805(3) .0306(9) Uani ? ? 1.00000 ? ?
O12 .31537(9) .23085(15) -.1654(3) .0327(10) Uani ? ? 1.00000 ? ?
N1 .34442(10) .48710(18) .0994(3) .0259(10) Uani ? ? 1.00000 ? ?
N2 .31591(10) .17498(17) .2102(3) .0255(10) Uani ? ? 1.00000 ? ?
C1 .21706(13) .30906(19) .2862(4) .0283(13) Uani ? ? 1.00000 ? ?
C2 .38007(12) .4258(2) .1797(4) .0251(12) Uani ? ? 1.00000 ? ?
C3 .42796(12) .4602(2) .2854(4) .0296(13) Uani ? ? 1.00000 ? ?
C4 .43547(13) .5478(2) .3026(4) .0330(14) Uani ? ? 1.00000 ? ?
C5 .39657(15) .6071(2) .2180(5) .0346(14) Uani ? ? 1.00000 ? ?
C6 .35132(13) .5745(2) .1168(4) .0316(13) Uani ? ? 1.00000 ? ?
C7 .21953(12) .39037(19) -.1965(4) .0247(12) Uani ? ? 1.00000 ? ?
C8 .20616(13) .4681(2) -.3034(5) .0302(13) Uani ? ? 1.00000 ? ?
C9 .15793(15) .4773(2) -.4118(5) .0348(14) Uani ? ? 1.00000 ? ?
C10 .12150(15) .4097(3) -.4239(5) .0399(16) Uani ? ? 1.00000 ? ?
C11 .36367(14) .1658(2) .3219(5) .0370(15) Uani ? ? 1.00000 ? ?
H1 .20428 .32773 .39374 .026(9) Uiso ? ? 1.00000 ? ?
H3 .45486 .42142 .34431 .041(11) Uiso ? ? 1.00000 ? ?
H4 .46517 .56837 .36297 .050(13) Uiso ? ? 1.00000 ? ?
H5 .40201 .66857 .23149 .029(9) Uiso ? ? 1.00000 ? ?
H6 .32124 .60740 .06261 .038(11) Uiso ? ? 1.00000 ? ?
H8 .23170 .50652 -.28377 .040(11) Uiso ? ? 1.00000 ? ?
H9 .14159 .51762 -.50460 .025(9) Uiso ? ? 1.00000 ? ?
H10 .08674 .41603 -.49991 .037(11) Uiso ? ? 1.00000 ? ?
H11 .38862 .22037 .33576 .040(11) Uiso ? ? 1.00000 ? ?
H1' .31541 .46660 .02972 .018(8) Uiso ? ? 1.00000 ? ?
C31 .4803(4) .2109(7) -.0315(13) .056(3) Uiso ? ? .51(3) ? ?
C32 .4410(5) .1555(9) -.044(2) .075(4) Uiso ? ? .51(3) ? ?
N3 .5118(7) .2603(12) -.033(2) .100(5) Uiso ? ? .51(3) ? ?
H321 .45071 .11310 .06040 .11800 Uiso ? ? .51(3) ? ?
H322 .41020 .19106 -.02101 .11800 Uiso ? ? .51(3) ? ?
H323 .43234 .12701 -.16769 .11800 Uiso ? ? .51(3) ? ?
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1'
H 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Cu .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1'
N .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1'
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
O2 Cu O4 . . 94.92(9) yes
O2 Cu O11 . . 95.93(9) yes
O2 Cu O12 . . 95.61(9) yes
O2 Cu N2 . . 95.18(10) yes
O4 Cu O11 . . 89.55(9) yes
O4 Cu O12 . . 89.76(9) yes
O4 Cu N2 . . 169.82(10) yes
O11 Cu O12 . . 168.46(10) yes
O11 Cu N2 . . 88.11(10) yes
O12 Cu N2 . . 90.56(9) yes
Cu O2 C2 . . 129.0(2) yes
Cu O4 C7 . . 130.4(2) yes
Cu O11 C1 . . 121.77(19) yes
Cu O12 C1 . 7_555 122.2(2) yes
C2 N1 C6 . . 125.0(3) yes
Cu N2 C11 . . 120.7(2) yes
Cu N2 C7 . 7_555 119.0(2) yes
C7 N2 C11 7_555 . 120.3(3) yes
C2 N1 H1' . . 115.60 no
C6 N1 H1' . . 119.35 no
O11 C1 O12 . 7_555 127.4(3) yes
N1 C2 C3 . . 114.9(3) yes
O2 C2 C3 . . 124.1(3) yes
O2 C2 N1 . . 121.0(3) yes
C2 C3 C4 . . 120.6(3) no
C3 C4 C5 . . 121.3(3) no
C4 C5 C6 . . 118.1(3) no
N1 C6 C5 . . 120.0(3) yes
N2 C7 C8 7_555 . 119.3(3) yes
O4 C7 C8 . . 120.1(3) yes
O4 C7 N2 . 7_555 120.7(3) yes
C7 C8 C9 . . 120.0(3) no
C8 C9 C10 . . 120.3(3) no
C9 C10 C11 . 7_555 118.1(3) no
N2 C11 C10 . 7_555 122.1(3) yes
O11 C1 H1 . . 117.95 no
O12 C1 H1 7_555 . 114.59 no
C2 C3 H3 . . 119.73 no
C4 C3 H3 . . 119.72 no
C3 C4 H4 . . 120.14 no
C5 C4 H4 . . 118.48 no
C4 C5 H5 . . 120.88 no
C6 C5 H5 . . 121.00 no
N1 C6 H6 . . 113.81 no
C5 C6 H6 . . 125.93 no
C7 C8 H8 . . 112.10 no
C9 C8 H8 . . 127.83 no
C8 C9 H9 . . 135.55 no
C10 C9 H9 . . 103.47 no
C9 C10 H10 . . 120.80 no
C11 C10 H10 7_555 . 121.09 no
N2 C11 H11 . . 117.07 no
C10 C11 H11 7_555 . 120.75 no
N3 C31 C32 . . 175.0(13) yes
C31 C32 H321 . . 106.90 no
C31 C32 H322 . . 105.77 no
C31 C32 H323 . . 113.10 no
H321 C32 H322 . . 109.29 no
H321 C32 H323 . . 111.82 no
H322 C32 H323 . . 109.73 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu O2 . . 2.146(2) yes
Cu O4 . . 1.966(2) yes
Cu O11 . . 2.004(2) yes
Cu O12 . . 1.988(2) yes
Cu N2 . . 1.985(3) yes
O2 C2 . . 1.249(4) yes
O4 C7 . . 1.290(4) yes
O11 C1 . . 1.256(4) yes
O12 C1 . 7_555 1.251(4) yes
N1 C2 . . 1.373(4) yes
N1 C6 . . 1.360(4) yes
N2 C11 . . 1.355(4) yes
N2 C7 . 7_555 1.359(4) yes
N1 H1' . . 0.8827 no
N3 C31 . . 1.12(2) yes
C2 C3 . . 1.435(4) no
C3 C4 . . 1.365(4) no
C4 C5 . . 1.414(5) no
C5 C6 . . 1.360(5) no
C7 C8 . . 1.428(4) no
C8 C9 . . 1.356(5) no
C9 C10 . . 1.403(6) no
C10 C11 . 7_555 1.388(5) no
C1 H1 . . 0.9421 no
C3 H3 . . 0.9569 no
C4 H4 . . 0.8729 no
C5 H5 . . 0.9592 no
C6 H6 . . 0.9535 no
C8 H8 . . 0.8831 no
C9 H9 . . 0.9493 no
C10 H10 . . 0.9709 no
C11 H11 . . 1.0568 no
C31 C32 . . 1.326(17) no
C32 H321 . . 0.9887 no
C32 H322 . . 1.0134 no
C32 H323 . . 0.9760 no
