#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/12/2011210.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_2011210
loop_
_publ_author_name
'Kani, Yoshiyuki'
'Tsuchimoto, Masanobu'
'Ohba, Shigeru'
'Matsushima, Hideaki'
'Tokii, Tadashi'
_publ_section_title
;catena-Poly[[tetrakis(μ-3,3-dimethylbutyrato-O:O')dicopper(II)]-μ-3,3-dimethylbutyrato-O:O'-[bis(2,6-dimethylpyridine-N)copper(II)]-μ-3,3-dimethylbutyrato-O:O']
 and
 tetrakis(μ-2,2-dimethylpropanoato-O:O')bis[(2,6-dimethylpyridine-N)copper(II)]
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              923
_journal_page_last               925
_journal_paper_doi               10.1107/S0108270100006697
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Cu3 (C6 H11 O2)6 (C7 H9 N)2]'
_chemical_formula_sum            'C50 H84 Cu3 N2 O12'
_chemical_formula_weight         1095.86
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                94.640(10)
_cell_angle_beta                 102.510(10)
_cell_angle_gamma                109.320(10)
_cell_formula_units_Z            1
_cell_length_a                   12.525(2)
_cell_length_b                   12.736(2)
_cell_length_c                   10.033(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     1454.1(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1993)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1999)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC-7R'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .021
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6956
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  .753
_exptl_absorpt_correction_T_min  .472
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Coppens et al., 1965)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .1
_refine_diff_density_max         .41
_refine_diff_density_min         -.61
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     304
_refine_ls_number_reflns         6651
_refine_ls_R_factor_gt           .045
_refine_ls_shift/su_max          .006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/{σ²Fo² + [0.05(Fo² + 2Fc²)/3]²}'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .115
_reflns_number_gt                4193
_reflns_number_total             6651
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            gd1098.cif
_cod_data_source_block           I
_cod_database_code               2011210
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-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_occupancy
_atom_site_type_symbol
Cu1 .39771(3) -.01312(3) .02690(4) .03660(10) Uani 1.00 Cu
Cu2 0 0 0 .0373(2) Uani 1.00 Cu
O1 .4572(2) .1533(2) .0615(3) .0577(8) Uani 1.00 O
O2 .6285(2) .1745(2) .0140(3) .0549(8) Uani 1.00 O
O3 .3478(2) -.0095(2) -.1720(2) .0528(7) Uani 1.00 O
O4 .5191(2) .0105(2) -.2182(2) .0494(7) Uani 1.00 O
O5 .2223(2) -.0375(2) .0512(2) .0474(7) Uani 1.00 O
O6 .0631(2) -.0846(2) .1269(2) .0459(7) Uani 1.00 O
N1 .0861(2) .1482(2) .1369(3) .0476(8) Uani 1.00 N
C1 .5562(3) .2117(3) .0473(4) .0483(10) Uani 1.00 C
C2 .5913(4) .3390(3) .0746(5) .0670(10) Uani 1.00 C
C3 .6623(4) .3959(4) .2214(5) .0750(10) Uani 1.00 C
C4 .6890(6) .5217(4) .2334(7) .122(2) Uani 1.00 C
C5 .7745(6) .3749(6) .2594(8) .140(3) Uani 1.00 C
C6 .5900(7) .3501(6) .3214(7) .157(3) Uani 1.00 C
C7 .4136(3) .0026(3) -.2518(3) .0402(8) Uani 1.00 C
C8 .3630(3) .0112(3) -.4003(3) .0453(9) Uani 1.00 C
C9 .3677(3) .1309(3) -.4251(4) .0490(10) Uani 1.00 C
C10 .3247(4) .1264(4) -.5803(4) .0680(10) Uani 1.00 C
C11 .2911(5) .1686(4) -.3509(5) .087(2) Uani 1.00 C
C12 .4938(4) .2136(4) -.3737(5) .085(2) Uani 1.00 C
C13 .1618(3) -.0919(3) .1225(3) .0399(9) Uani 1.00 C
C14 .2032(3) -.1699(3) .2079(4) .0490(10) Uani 1.00 C
C15 .1138(3) -.2806(3) .2240(4) .0600(10) Uani 1.00 C
C16 .0335(5) -.3444(4) .0878(7) .107(2) Uani 1.00 C
C17 .0414(5) -.2575(5) .3207(6) .098(2) Uani 1.00 C
C18 .1813(5) -.3517(5) .2887(7) .111(2) Uani 1.00 C
C19 .1754(3) .2305(3) .1093(4) .0520(10) Uani 1.00 C
C20 .2279(4) .3344(4) .1951(5) .0750(10) Uani 1.00 C
C21 .1902(5) .3547(4) .3086(5) .082(2) Uani 1.00 C
C22 .1013(5) .2720(4) .3367(5) .076(2) Uani 1.00 C
C23 .0488(3) .1677(3) .2497(4) .0560(10) Uani 1.00 C
C24 .2145(3) .2074(3) -.0151(5) .0620(10) Uani 1.00 C
C25 -.0476(4) .0746(4) .2784(4) .0710(10) Uani 1.00 C
H1 .6373 .3698 .0123 .0800 Uiso 1.00 H
H2 .5211 .3564 .0558 .0800 Uiso 1.00 H
H3 .7307 .5576 .3269 .1458 Uiso 1.00 H
H4 .7362 .5516 .1720 .1458 Uiso 1.00 H
H5 .6170 .5357 .2089 .1458 Uiso 1.00 H
H6 .7581 .2951 .2520 .1679 Uiso 1.00 H
H7 .8216 .4049 .1978 .1679 Uiso 1.00 H
H8 .8162 .4109 .3528 .1679 Uiso 1.00 H
H9 .6327 .3875 .4140 .1881 Uiso 1.00 H
H10 .5175 .3633 .2976 .1881 Uiso 1.00 H
H11 .5738 .2705 .3157 .1881 Uiso 1.00 H
H12 .4059 -.0130 -.4570 .0543 Uiso 1.00 H
H13 .2825 -.0384 -.4281 .0543 Uiso 1.00 H
H14 .3273 .2000 -.5984 .0813 Uiso 1.00 H
H15 .3741 .1027 -.6271 .0813 Uiso 1.00 H
H16 .2457 .0738 -.6131 .0813 Uiso 1.00 H
H17 .3189 .1718 -.2531 .1046 Uiso 1.00 H
H18 .2935 .2420 -.3694 .1046 Uiso 1.00 H
H19 .2120 .1159 -.3829 .1046 Uiso 1.00 H
H20 .5214 .2160 -.2760 .1021 Uiso 1.00 H
H21 .5424 .1894 -.4214 .1021 Uiso 1.00 H
H22 .4970 .2874 -.3912 .1021 Uiso 1.00 H
H23 .2582 -.1893 .1670 .0588 Uiso 1.00 H
H24 .2426 -.1279 .2993 .0588 Uiso 1.00 H
H25 -.0096 -.3001 .0467 .1289 Uiso 1.00 H
H26 .0785 -.3599 .0277 .1289 Uiso 1.00 H
H27 -.0201 -.4141 .1012 .1289 Uiso 1.00 H
H28 .0930 -.2170 .4087 .1180 Uiso 1.00 H
H29 -.0021 -.2132 .2805 .1180 Uiso 1.00 H
H30 -.0118 -.3277 .3333 .1180 Uiso 1.00 H
H31 .1273 -.4214 .3015 .1329 Uiso 1.00 H
H32 .2264 -.3672 .2287 .1329 Uiso 1.00 H
H33 .2329 -.3112 .3767 .1329 Uiso 1.00 H
H34 .2910 .3923 .1744 .0897 Uiso 1.00 H
H35 .2262 .4267 .3681 .0989 Uiso 1.00 H
H36 .0743 .2853 .4168 .0914 Uiso 1.00 H
H37 .2397 .1442 -.0088 .0750 Uiso 1.00 H
H38 .1507 .1906 -.0961 .0750 Uiso 1.00 H
H39 .2783 .2725 -.0212 .0750 Uiso 1.00 H
H40 -.0655 .0994 .3610 .0851 Uiso 1.00 H
H41 -.1159 .0533 .2019 .0851 Uiso 1.00 H
H42 -.0238 .0109 .2907 .0851 Uiso 1.00 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu .320 1.265
;International Tables for Crystallography
(1992, Vol. C)
;
C C .003 .002
;International Tables for Crystallography
(1992, Vol. C)
;
H H .000 .000
;International Tables for Crystallography
(1992, Vol. C)
;
O O .011 .006
;International Tables for Crystallography
(1992, Vol. C)
;
N N .006 .003
;International Tables for Crystallography
(1992, Vol. C)
;
Na Na .036 .025
;International Tables for Crystallography
(1992, Vol. C)
;
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
Cu1 Cu1 O1 2_655 . 84.20(10) no
Cu1 Cu1 O2 2_655 2_655 83.60(10) no
Cu1 Cu1 O3 2_655 . 83.30(10) no
Cu1 Cu1 O4 2_655 2_655 84.40(10) no
Cu1 Cu1 O5 2_655 . 174.90(10) no
O1 Cu1 O2 . 2_655 167.70(10) yes
O1 Cu1 O3 . . 88.90(10) no
O1 Cu1 O4 . 2_655 89.10(10) no
O1 Cu1 O5 . . 96.70(10) no
O2 Cu1 O3 2_655 . 90.30(10) no
O2 Cu1 O4 2_655 2_655 89.10(10) no
O2 Cu1 O5 2_655 . 95.60(10) no
O3 Cu1 O4 . 2_655 167.70(10) yes
O3 Cu1 O5 . . 91.70(10) no
O4 Cu1 O5 2_655 . 100.70(10) no
O6 Cu2 O6 . 2_555 180.0 no
O6 Cu2 N1 . . 92.20(10) yes
O6 Cu2 N1 . 2_555 87.80(10) no
O6 Cu2 N1 2_555 . 87.80(10) no
O6 Cu2 N1 2_555 2_555 92.20(10) no
N1 Cu2 N1 . 2_555 180.0 no
Cu1 O1 C1 . . 122.4(2) no
Cu1 O2 C1 2_655 . 124.0(2) no
Cu1 O3 C7 . . 124.2(2) no
Cu1 O4 C7 2_655 . 122.7(2) no
Cu1 O5 C13 . . 134.1(2) yes
Cu2 O6 C13 . . 117.8(2) no
Cu2 N1 C19 . . 120.1(2) no
Cu2 N1 C23 . . 120.3(2) no
C19 N1 C23 . . 119.4(3) no
O1 C1 O2 . . 125.9(3) yes
O1 C1 C2 . . 117.4(3) no
O2 C1 C2 . . 116.7(3) no
C1 C2 C3 . . 115.2(3) no
C1 C2 H1 . . 108.0 no
C1 C2 H2 . . 108.0 no
C3 C2 H1 . . 108.0 no
C3 C2 H2 . . 108.0 no
H1 C2 H2 . . 109.5 no
C2 C3 C4 . . 109.1(4) no
C2 C3 C5 . . 111.9(4) no
C2 C3 C6 . . 108.8(4) no
C4 C3 C5 . . 109.1(5) no
C4 C3 C6 . . 108.9(5) no
C5 C3 C6 . . 109.0(6) no
C3 C4 H3 . . 109.5 no
C3 C4 H4 . . 109.5 no
C3 C4 H5 . . 109.5 no
H3 C4 H4 . . 109.5 no
H3 C4 H5 . . 109.4 no
H4 C4 H5 . . 109.4 no
C3 C5 H6 . . 109.5 no
C3 C5 H7 . . 109.5 no
C3 C5 H8 . . 109.5 no
H6 C5 H7 . . 109.4 no
H6 C5 H8 . . 109.4 no
H7 C5 H8 . . 109.5 no
C3 C6 H9 . . 109.5 no
C3 C6 H10 . . 109.5 no
C3 C6 H11 . . 109.5 no
H9 C6 H10 . . 109.4 no
H9 C6 H11 . . 109.5 no
H10 C6 H11 . . 109.4 no
O3 C7 O4 . . 125.3(3) yes
O3 C7 C8 . . 117.4(3) no
O4 C7 C8 . . 117.3(3) no
C7 C8 C9 . . 114.9(3) no
C7 C8 H12 . . 108.1 no
C7 C8 H13 . . 108.1 no
C9 C8 H12 . . 108.1 no
C9 C8 H13 . . 108.1 no
H12 C8 H13 . . 109.5 no
C8 C9 C10 . . 107.9(3) no
C8 C9 C11 . . 110.7(3) no
C8 C9 C12 . . 109.5(3) no
C10 C9 C11 . . 109.8(3) no
C10 C9 C12 . . 109.3(3) no
C11 C9 C12 . . 109.7(4) no
C9 C10 H14 . . 109.5 no
C9 C10 H15 . . 109.5 no
C9 C10 H16 . . 109.5 no
H14 C10 H15 . . 109.5 no
H14 C10 H16 . . 109.5 no
H15 C10 H16 . . 109.5 no
C9 C11 H17 . . 109.5 no
C9 C11 H18 . . 109.5 no
C9 C11 H19 . . 109.5 no
H17 C11 H18 . . 109.5 no
H17 C11 H19 . . 109.4 no
H18 C11 H19 . . 109.5 no
C9 C12 H20 . . 109.5 no
C9 C12 H21 . . 109.5 no
C9 C12 H22 . . 109.5 no
H20 C12 H21 . . 109.4 no
H20 C12 H22 . . 109.5 no
H21 C12 H22 . . 109.5 no
O5 C13 O6 . . 121.9(3) yes
O5 C13 C14 . . 120.4(3) no
O6 C13 C14 . . 117.7(3) no
C13 C14 C15 . . 119.4(3) no
C13 C14 H23 . . 106.9 no
C13 C14 H24 . . 106.9 no
C15 C14 H23 . . 106.9 no
C15 C14 H24 . . 106.9 no
H23 C14 H24 . . 109.5 no
C14 C15 C16 . . 111.6(4) no
C14 C15 C17 . . 110.3(4) no
C14 C15 C18 . . 107.6(3) no
C16 C15 C17 . . 109.4(4) no
C16 C15 C18 . . 109.1(4) no
C17 C15 C18 . . 108.7(4) no
C15 C16 H25 . . 109.5 no
C15 C16 H26 . . 109.5 no
C15 C16 H27 . . 109.5 no
H25 C16 H26 . . 109.5 no
H25 C16 H27 . . 109.5 no
H26 C16 H27 . . 109.5 no
C15 C17 H28 . . 109.5 no
C15 C17 H29 . . 109.5 no
C15 C17 H30 . . 109.5 no
H28 C17 H29 . . 109.5 no
H28 C17 H30 . . 109.5 no
H29 C17 H30 . . 109.5 no
C15 C18 H31 . . 109.5 no
C15 C18 H32 . . 109.5 no
C15 C18 H33 . . 109.5 no
H31 C18 H32 . . 109.4 no
H31 C18 H33 . . 109.5 no
H32 C18 H33 . . 109.4 no
N1 C19 C20 . . 120.6(4) no
N1 C19 C24 . . 118.5(3) no
C20 C19 C24 . . 120.9(4) no
C19 C20 C21 . . 120.2(4) no
C19 C20 H34 . . 119.9 no
C21 C20 H34 . . 119.9 no
C20 C21 C22 . . 119.2(4) no
C20 C21 H35 . . 120.4 no
C22 C21 H35 . . 120.4 no
C21 C22 C23 . . 120.3(4) no
C21 C22 H36 . . 119.9 no
C23 C22 H36 . . 119.9 no
N1 C23 C22 . . 120.3(4) no
N1 C23 C25 . . 117.9(3) no
C22 C23 C25 . . 121.8(4) no
C19 C24 H37 . . 109.5 no
C19 C24 H38 . . 109.5 no
C19 C24 H39 . . 109.5 no
H37 C24 H38 . . 109.5 no
H37 C24 H39 . . 109.5 no
H38 C24 H39 . . 109.5 no
C23 C25 H40 . . 109.5 no
C23 C25 H41 . . 109.5 no
C23 C25 H42 . . 109.5 no
H40 C25 H41 . . 109.5 no
H40 C25 H42 . . 109.5 no
H41 C25 H42 . . 109.5 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
Cu1 Cu1 . 2_655 2.6520(10) yes
Cu1 O1 . . 1.972(3) yes
Cu1 O2 . 2_655 1.965(2) yes
Cu1 O3 . . 1.967(2) yes
Cu1 O4 . 2_655 1.967(2) yes
Cu1 O5 . . 2.185(2) yes
Cu2 O5 . . 2.923(2) yes
Cu2 O6 . . 1.938(2) yes
Cu2 O6 . 2_555 1.938(2) no
Cu2 N1 . . 2.050(3) yes
Cu2 N1 . 2_555 2.050(3) no
O1 C1 . . 1.263(4) no
O2 C1 . . 1.243(4) no
O3 C7 . . 1.252(4) no
O4 C7 . . 1.259(4) no
O5 C13 . . 1.238(4) no
O6 C13 . . 1.280(3) no
N1 C19 . . 1.353(4) no
N1 C23 . . 1.350(4) no
C1 C2 . . 1.516(5) no
C2 C3 . . 1.523(6) no
C2 H1 . . .960 no
C2 H2 . . .960 no
C3 C4 . . 1.513(7) no
C3 C5 . . 1.492(8) no
C3 C6 . . 1.518(7) no
C4 H3 . . .960 no
C4 H4 . . .960 no
C4 H5 . . .961 no
C5 H6 . . .961 no
C5 H7 . . .960 no
C5 H8 . . .960 no
C6 H9 . . .960 no
C6 H10 . . .961 no
C6 H11 . . .960 no
C7 C8 . . 1.515(4) no
C8 C9 . . 1.548(5) no
C8 H12 . . .960 no
C8 H13 . . .960 no
C9 C10 . . 1.523(5) no
C9 C11 . . 1.503(5) no
C9 C12 . . 1.526(6) no
C10 H14 . . .960 no
C10 H15 . . .960 no
C10 H16 . . .960 no
C11 H17 . . .960 no
C11 H18 . . .960 no
C11 H19 . . .960 no
C12 H20 . . .960 no
C12 H21 . . .960 no
C12 H22 . . .960 no
C13 C14 . . 1.509(4) no
C14 C15 . . 1.529(5) no
C14 H23 . . .960 no
C14 H24 . . .960 no
C15 C16 . . 1.491(7) no
C15 C17 . . 1.537(6) no
C15 C18 . . 1.523(6) no
C16 H25 . . .960 no
C16 H26 . . .960 no
C16 H27 . . .960 no
C17 H28 . . .960 no
C17 H29 . . .960 no
C17 H30 . . .960 no
C18 H31 . . .960 no
C18 H32 . . .960 no
C18 H33 . . .960 no
C19 C20 . . 1.385(6) no
C19 C24 . . 1.478(6) no
C20 C21 . . 1.361(7) no
C20 H34 . . .960 no
C21 C22 . . 1.355(7) no
C21 H35 . . .960 no
C22 C23 . . 1.395(6) no
C22 H36 . . .960 no
C23 C25 . . 1.485(6) no
C24 H37 . . .960 no
C24 H38 . . .960 no
C24 H39 . . .960 no
C25 H40 . . .960 no
C25 H41 . . .960 no
C25 H42 . . .960 no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
Cu1 Cu1 2.6515(9) 2_655
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
_geom_torsion_publ_flag
Cu1 O5 C13 O6 173.8(2) yes
Cu2 O6 C13 O5 7.7(4) yes
