#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/37/2103751.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_2103751
loop_
_publ_author_name
'Yasui, Masanori'
'Ishikawa, Yoshimitsu'
'Ishida, Takayuki'
'Nogami, Takashi'
'Iwasaki, Fujiko'
_publ_section_title
;
 Bis(hfac)-copper(II) complexes bridged by pyrimidines showing magnetic
 interactions
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              772
_journal_page_last               779
_journal_paper_doi               10.1107/S0108768101013568
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         'Cu, 2(C5 H1 F6 O2), C4 H4 N2'
_chemical_formula_sum            'C14 H6 Cu F12 N2 O4'
_chemical_formula_weight         557.75
_chemical_name_common
;
bis(1,1,1,5,5,5-hexafluoropentane-2,4-dionato)-bispyrimidinecopper(II)
;
_chemical_name_systematic
;
catena-bis(1,1,1,5,5,5-hexafluoropentane-2,4-dionato)[m-pyrimidine-N1:N3]
copper(II)
;
_space_group_IT_number           110
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4bw -2c'
_symmetry_space_group_name_H-M   'I 41 c d'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   18.3757(17)
_cell_length_b                   18.3757
_cell_length_c                   22.137(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    120
_cell_measurement_theta_max      17.4
_cell_measurement_theta_min      13.2
_cell_volume                     7474.9(12)
_computing_cell_refinement       'AFC Control Software (Rigaku, 1994)'
_computing_data_collection       'AFC Control Software (Rigaku, 1994)'
_computing_data_reduction
'teXsan, (Molecular Science Corporation, 1992)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1972)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full .511
_diffrn_measured_fraction_theta_max .511
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0294
_diffrn_reflns_av_sigmaI/netI    .0335
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4317
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        .93
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.312
_exptl_absorpt_correction_T_max  .753
_exptl_absorpt_correction_T_min  .724
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Coppens, et al. 1965)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       pillar
_exptl_crystal_F_000             4368
_exptl_crystal_size_max          .330
_exptl_crystal_size_mid          .250
_exptl_crystal_size_min          .250
_refine_diff_density_max         .595
_refine_diff_density_min         -.360
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   .012(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         2210
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          .0342
_refine_ls_R_factor_gt           .0296
_refine_ls_shift/su_max          .003
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0433P)²+8.5189P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .0827
_reflns_number_gt                2008
_reflns_number_total             2210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            oa0036.cif
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      'I 41 c d     '
_cod_original_formula_sum        'C14 H6 Cu F12 N2 O4 '
_cod_database_code               2103751
_cod_database_fobs_code          2103751
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, z+1/2'
'y, -x+1/2, z+1/4'
'y, x+1/2, z+3/4'
'-x, -y, z'
'x, -y, z+1/2'
'-y, x+1/2, z+1/4'
'-y, -x+1/2, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1'
'y+1/2, -x+1, z+3/4'
'y+1/2, x+1, z+5/4'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1'
'-y+1/2, x+1, z+3/4'
'-y+1/2, -x+1, z+5/4'
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_occupancy
_atom_site_type_symbol
Cu .16515(2) .24964(3) .00156(3) .01554(12) Uani d 1 Cu
O1 .16737(16) .35086(16) .02827(14) .0179(6) Uani d 1 O
O2 .07080(17) .28536(16) -.06342(14) .0233(6) Uani d 1 O
O3 .08203(15) .22797(16) .05622(14) .0207(6) Uani d 1 O
O4 .16951(17) .14794(17) -.02323(13) .0185(6) Uani d 1 O
N1 .2384(2) .27075(19) -.06480(15) .0167(7) Uani d 1 N
N2 .2712(2) .24742(18) -.16681(15) .0177(7) Uani d 1 N
C1 .1175(2) .3989(2) .02275(18) .0159(8) Uani d 1 C
C2 .0550(2) .3983(2) -.0113(2) .0205(9) Uani d 1 C
C3 .0370(2) .3419(2) -.0520(2) .0197(8) Uani d 1 C
C4 .1347(2) .4673(2) .0593(2) .0229(9) Uani d 1 C
C5 -.0364(3) .3515(3) -.0849(2) .0310(10) Uani d 1 C
C6 .0418(2) .1733(2) .0500(2) .0180(8) Uani d 1 C
C7 .0547(2) .1110(2) .0156(2) .0206(8) Uani d 1 C
C8 .1184(2) .1031(2) -.01714(18) .0175(8) Uani d 1 C
C9 -.0292(3) .1774(3) .0860(3) .0338(11) Uani d 1 C
C10 .1327(2) .0300(2) -.0492(2) .0231(9) Uani d 1 C
C11 .2289(2) .2390(2) -.1187(2) .0199(8) Uani d 1 C
C12 .3282(2) .2937(2) -.1608(2) .0211(8) Uani d 1 C
C13 .3417(2) .3291(2) -.1073(2) .0249(9) Uani d 1 C
C14 .2946(2) .3168(2) -.0594(2) .0216(8) Uani d 1 C
F1 .1895(2) .5031(2) .03502(19) .0666(12) Uani d 1 F
F2 .07887(19) .5128(2) .0643(2) .0630(13) Uani d 1 F
F3 .1539(2) .45232(18) .11532(15) .0438(8) Uani d 1 F
F4 -.0513(2) .42101(17) -.09664(18) .0622(12) Uani d 1 F
F5 -.09090(17) .3267(3) -.05084(18) .0642(11) Uani d 1 F
F6 -.0383(2) .31640(19) -.13656(16) .0484(9) Uani d 1 F
F7 -.06923(19) .2327(3) .0655(2) .0749(14) Uani d 1 F
F8 -.01904(19) .1885(2) .14359(15) .0524(9) Uani d 1 F
F9 -.06951(18) .1175(2) .0812(2) .0678(13) Uani d 1 F
F10 .1571(2) .04061(19) -.10498(16) .0514(10) Uani d 1 F
F11 .1806(3) -.0083(2) -.02059(17) .0669(12) Uani d 1 F
F12 .07328(19) -.0106(2) -.0541(2) .0627(13) Uani d 1 F
H2 .025(2) .439(2) -.013(2) .017(11) Uiso d 1 H
H7 .019(3) .077(3) .004(3) .032(14) Uiso d 1 H
H11 .187(3) .206(3) -.120(3) .036(14) Uiso d 1 H
H12 .354(2) .300(3) -.197(2) .018(11) Uiso d 1 H
H13 .382(2) .363(2) -.107(2) .018(11) Uiso d 1 H
H14 .305(3) .343(3) -.020(2) .022(12) 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 .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu .3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 '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
O1 Cu O2 . . 86.25(12) yes
O1 Cu O3 . . 91.29(12) yes
O1 Cu O4 . . 176.22(11) yes
O1 Cu N1 . . 91.33(13) yes
O1 Cu N2 . 3 84.84(13) yes
O2 Cu O4 . . 97.24(12) yes
O2 Cu O3 . . 82.04(11) yes
O2 Cu N1 . . 89.58(13) yes
O2 Cu N2 . 3 167.66(12) yes
O3 Cu O4 . . 90.62(13) yes
O3 Cu N1 . . 171.04(14) yes
O3 Cu N2 . 3 89.63(12) yes
O4 Cu N1 . . 87.27(13) yes
O4 Cu N2 . 3 91.92(13) yes
N1 Cu N2 . 3 99.14(11) yes
Cu O1 C1 . . 127.8(3) no
Cu O2 C3 . . 118.7(3) no
Cu O3 C6 . . 123.0(3) no
Cu O4 C8 . . 124.6(3) no
Cu N1 C11 . . 118.4(3) no
Cu N1 C14 . . 124.5(3) no
C11 N1 C14 . . 117.0(4) no
Cu N2 C11 15_544 . 116.1(3) no
Cu N2 C12 15_544 . 126.5(3) no
C11 N2 C12 . . 116.5(4) no
O1 C1 C2 . . 130.3(4) no
O1 C1 C4 . . 111.6(4) no
C2 C1 C4 . . 118.0(4) no
C1 C2 C3 . . 123.5(4) no
O2 C3 C2 . . 129.0(4) no
O2 C3 C5 . . 116.0(4) no
C2 C3 C5 . . 115.0(4) no
C1 C4 F1 . . 110.7(4) no
C1 C4 F2 . . 113.7(4) no
C1 C4 F3 . . 112.4(4) no
F1 C4 F2 . . 108.1(4) no
F1 C4 F3 . . 106.4(4) no
F2 C4 F3 . . 105.0(4) no
C3 C5 F4 . . 112.5(4) no
C3 C5 F5 . . 110.5(4) no
C3 C5 F6 . . 112.3(4) no
F4 C5 F5 . . 106.5(5) no
F4 C5 F6 . . 107.1(4) no
F5 C5 F6 . . 107.7(4) no
O3 C6 C7 . . 128.1(4) no
O3 C6 C9 . . 113.9(4) no
C7 C6 C9 . . 118.0(4) no
C6 C7 C6 . . 121.1(4) no
O4 C8 C7 . . 128.2(4) no
O4 C8 C10 . . 113.3(4) no
C7 C8 C10 . . 118.5(4) no
F7 C9 F8 . . 107.1(5) no
F7 C9 F9 . . 107.2(5) no
F8 C9 F9 . . 106.7(5) no
C6 C9 F7 . . 109.3(4) no
C6 C9 F8 . . 113.2(4) no
C6 C9 F9 . . 113.0(4) no
C8 C10 F10 . . 111.0(4) no
C8 C10 F11 . . 111.4(4) no
C8 C10 F12 . . 112.8(4) no
F10 C10 F11 . . 107.7(4) no
F10 C10 F12 . . 106.5(4) no
F11 C10 F12 . . 107.1(5) no
N2 C11 N1 . . 126.0(3) no
N2 C12 C13 . . 121.4(4) no
C12 C13 C14 . . 118.0(4) no
N1 C14 C13 . . 121.0(4) no
C1 C2 H2 . . 120(3) no
C3 C2 H2 . . 116(3) no
C8 C7 H7 . . 112(3) no
C6 C7 H7 . . 125(3) no
N2 C11 H11 . . 120(4) no
N1 C11 H11 . . 114(4) no
N2 C12 H12 . . 113(3) no
C13 C12 H12 . . 126(3) no
C12 C13 H13 . . 117(3) no
C14 C13 H13 . . 125(3) no
N1 C14 H14 . . 121(3) no
C13 C14 H14 . . 118(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
Cu O1 . 1.952(3) yes
Cu O2 . 2.346(3) yes
Cu O3 . 1.989(3) yes
Cu O4 . 1.949(3) yes
Cu N1 . 2.029(4) yes
Cu N2 3 2.387(3) yes
O1 C1 . 1.278(5) no
O2 C3 . 1.237(5) no
O3 C6 . 1.255(5) no
O4 C8 . 1.256(6) no
N1 C11 . 1.339(6) no
N1 C14 . 1.341(5) no
N2 C11 . 1.327(6) no
N2 C12 . 1.357(5) no
N2 Cu 15_544 2.387(3) no
C1 C2 . 1.373(6) no
C1 C4 . 1.529(6) no
C2 C3 . 1.411(6) no
C3 C5 . 1.542(6) no
C4 F1 . 1.318(6) no
C4 F2 . 1.328(5) no
C4 F3 . 1.319(6) no
C5 F4 . 1.332(6) no
C5 F5 . 1.334(7) no
C5 F6 . 1.314(6) no
C6 C7 . 1.394(6) no
C6 C9 . 1.532(6) no
C7 C8 . 1.384(6) no
C8 C10 . 1.540(6) no
C9 F7 . 1.334(6) no
C9 F8 . 1.305(7) no
C9 F9 . 1.330(6) no
C10 F10 . 1.329(6) no
C10 F11 . 1.292(6) no
C10 F12 . 1.327(5) no
C12 C13 . 1.373(6) no
C13 C14 . 1.388(6) no
C2 H2 . .93(4) no
C7 H7 . .93(5) no
C11 H11 . .98(5) no
C12 H12 . .95(5) no
C13 H13 . .97(4) no
C14 H14 . 1.01(5) no
