#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/37/2103752.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_2103752
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), C5 H6 N2'
_chemical_formula_sum            'C15 H8 Cu F12 N2 O4'
_chemical_formula_weight         571.78
_chemical_name_common
;
bis(1,1,1,5,5,5-hexafluoropentane-2,4-dionato)-bis(4-methylpyrimidine)
copper(II)
;
_chemical_name_systematic
;
catena-bis(1,1,1,5,5,5-hexafluoropentane-2,4-dionato)[m-4-methylpyrimidine-
N1:N3]copper(II)
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   19.253(8)
_cell_length_b                   19.253
_cell_length_c                   22.380(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      17.4
_cell_measurement_theta_min      13.5
_cell_volume                     8296(5)
_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    'SAPI91 (Fan Hai-Fu. 1991)'
_diffrn_ambient_temperature      294
_diffrn_measured_fraction_theta_full .487
_diffrn_measured_fraction_theta_max .487
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0280
_diffrn_reflns_av_sigmaI/netI    .0674
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5031
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        -2.41
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.185
_exptl_absorpt_correction_T_max  .795
_exptl_absorpt_correction_T_min  .764
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4496
_exptl_crystal_size_max          .200
_exptl_crystal_size_mid          .200
_exptl_crystal_size_min          .200
_refine_diff_density_max         .546
_refine_diff_density_min         -.367
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          .1200
_refine_ls_R_factor_gt           .0527
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0781P)²+8.0262P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1796
_reflns_number_gt                2602
_reflns_number_total             4747
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            oa0036.cif
_cod_data_source_block           2a
_cod_original_sg_symbol_H-M      'I 41/a       '
_cod_original_formula_sum        'C15 H8 Cu1 F12 N2 O4'
_cod_database_code               2103752
_cod_database_fobs_code          2103752
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'
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_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Cu1 .16103(3) .49044(3) .24405(2) .0513(2) Uani d . 1 Cu
O1 .16593(16) .39407(15) .27043(14) .0539(8) Uani d . 1 O
O2 .06535(19) .46005(18) .19108(15) .0663(9) Uani d . 1 O
O3 .09356(18) .51207(18) .30904(14) .0625(9) Uani d . 1 O
O4 .15940(18) .58746(16) .21899(15) .0592(8) Uani d . 1 O
N1 .22735(19) .47177(17) .17575(15) .0462(8) Uani d . 1 N
N2 .25679(19) .4916(2) .07441(16) .0520(9) Uani d . 1 N
C1 .1185(2) .3487(2) .26718(19) .0475(10) Uani d . 1 C
C2 .0557(3) .3509(3) .2385(2) .0563(12) Uani d . 1 C
C3 .0341(2) .4069(3) .2026(2) .0567(11) Uani d . 1 C
C4 .1377(3) .2812(3) .2995(3) .0634(13) Uani d . 1 C
C5 -.0394(3) .4004(4) .1760(3) .0847(18) Uani d . 1 C
C6 .0552(3) .5639(3) .3093(2) .0615(12) Uani d . 1 C
C7 .0603(3) .6227(3) .2728(3) .0666(14) Uani d . 1 C
C8 .1132(3) .6307(3) .2325(2) .0594(12) Uani d . 1 C
C9 -.0020(4) .5621(4) .3559(3) .102(2) Uani d . 1 C
C10 .1217(4) .7004(3) .2013(3) .0792(17) Uani d . 1 C
C11 .2200(2) .5035(2) .12341(18) .0512(11) Uani d . 1 C
C12 .2780(3) .4242(2) .1789(2) .0574(12) Uani d . 1 C
C13 .3189(3) .4091(3) .1313(2) .0611(13) Uani d . 1 C
C14 .3067(2) .4427(2) .0777(2) .0534(11) Uani d . 1 C
C15 .3453(3) .4273(3) .0224(3) .0808(17) Uani d . 1 C
F1 .1720(2) .29227(19) .34908(18) .1113(15) Uani d . 1 F
F2 .1769(3) .2427(2) .2656(2) .1368(19) Uani d . 1 F
F3 .0843(2) .24209(19) .3137(2) .1128(15) Uani d . 1 F
F4 -.0598(2) .3362(3) .1668(3) .148(2) Uani d . 1 F
F5 -.0845(2) .4284(4) .2109(3) .192(3) Uani d . 1 F
F6 -.0445(3) .4305(3) .1243(2) .1412(19) Uani d . 1 F
F7 -.0380(2) .5056(3) .3536(3) .149(2) Uani d . 1 F
F8 -.0453(4) .6133(4) .3530(3) .203(4) Uani d . 1 F
F9 .0243(3) .5637(4) .40901(19) .169(3) Uani d . 1 F
F10 .0745(3) .7437(2) .2113(4) .185(3) Uani d . 1 F
F11 .1807(3) .7306(2) .2215(2) .1148(14) Uani d . 1 F
F12 .1331(3) .6939(2) .14370(18) .1154(15) Uani d . 1 F
H2 .033(3) .313(3) .241(2) .083(19) Uiso d . 1 H
H7 .031(3) .655(3) .277(2) .059(14) Uiso d . 1 H
H11 .1857 .5373 .1209 .061 Uiso calc R 1 H
H12 .2853 .4009 .2148 .069 Uiso calc R 1 H
H13 .3545 .3766 .1346 .073 Uiso calc R 1 H
H151 .3287 .4565 -.0093 .121 Uiso calc R 1 H
H152 .3386 .3794 .0117 .121 Uiso calc R 1 H
H153 .3939 .4358 .0287 .121 Uiso calc R 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'
O O .0106 .0060 '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'
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 Cu1 O2 . . 87.25(12) yes
O1 Cu1 O3 . . 90.54(14) yes
O1 Cu1 O4 . . 177.92(14) yes
O1 Cu1 N1 . . 91.67(14) yes
O1 Cu1 N2 . 3 82.63(12) yes
O2 Cu1 O3 . . 84.61(15) yes
O2 Cu1 O4 . . 94.80(14) yes
O2 Cu1 N1 . . 94.12(14) yes
O2 Cu1 N2 . 3 166.50(12) yes
O3 Cu1 O4 . . 89.96(14) yes
O3 Cu1 N1 . . 177.39(14) yes
O3 Cu1 N2 . 3 86.58(14) yes
O4 Cu1 N1 . . 87.88(14) yes
O4 Cu1 N2 . 3 95.39(14) yes
N1 Cu1 N2 . 3 95.08(14) yes
Cu1 O1 C1 . . 127.2(3) no
Cu1 O2 C3 . . 120.6(3) no
Cu1 O3 C6 . . 123.9(3) no
Cu1 O4 C8 . . 125.3(3) no
Cu1 N1 C11 . . 121.2(3) no
Cu1 N1 C12 . . 122.7(3) no
C11 N1 C12 . . 116.0(4) no
Cu1 N2 C11 8_454 . 112.4(3) no
Cu1 N2 C14 8_454 . 128.6(3) no
C11 N2 C14 . . 117.1(4) no
O1 C1 C2 . . 130.0(4) no
O1 C1 C4 . . 112.5(4) no
C2 C1 C4 . . 117.5(4) no
C1 C2 C3 . . 123.5(5) no
C1 C2 H2 . . 113(4) no
C3 C2 H2 . . 123(4) no
O2 C3 C2 . . 128.3(5) no
O2 C3 C5 . . 116.1(5) no
C2 C3 C5 . . 115.5(5) no
C1 C4 F1 . . 112.6(4) no
C1 C4 F2 . . 110.3(4) no
C1 C4 F3 . . 114.3(4) no
F1 C4 F2 . . 107.1(5) no
F1 C4 F3 . . 106.5(5) no
F2 C4 F3 . . 105.5(5) no
C3 C5 F4 . . 114.2(5) no
C3 C5 F5 . . 110.6(6) no
C3 C5 F6 . . 112.3(6) no
F4 C5 F5 . . 106.7(7) no
F4 C5 F6 . . 104.9(6) no
F5 C5 F6 . . 107.7(6) no
O3 C6 C7 . . 127.3(5) no
O3 C6 C9 . . 114.6(5) no
C7 C6 C9 . . 118.1(5) no
C8 C7 C6 . . 121.9(5) no
C6 C7 H7 . . 119(4) no
C8 C7 H7 . . 119(4) no
O4 C8 C7 . . 127.6(5) no
O4 C8 C10 . . 113.5(5) no
C7 C8 C10 . . 118.8(5) no
C6 C9 F7 . . 112.4(7) no
C6 C9 F8 . . 114.5(6) no
C6 C9 F9 . . 110.4(7) no
F7 C9 F8 . . 107.0(8) no
F7 C9 F9 . . 105.5(7) no
F8 C9 F9 . . 106.3(8) no
C8 C10 F10 . . 115.2(5) no
C8 C10 F12 . . 112.6(5) no
C8 C10 F11 . . 108.4(5) no
F10 C10 F12 . . 111.1(6) no
F10 C10 F11 . . 105.3(6) no
F11 C10 F12 . . 103.3(5) no
N1 C11 N2 . . 126.4(4) no
N1 C11 H11 . . 116.8 no
N2 C11 H11 . . 116.8 no
N1 C12 C13 . . 121.8(4) no
N1 C12 H12 . . 119.1 no
C13 C12 H12 . . 119.1 no
C12 C13 C14 . . 118.8(4) no
C12 C13 H13 . . 120.6 no
C14 C13 H13 . . 120.6 no
N2 C14 C13 . . 119.8(4) no
N2 C14 C15 . . 117.0(4) no
C13 C14 C15 . . 123.2(4) no
C14 C15 H151 . . 109.5 no
C14 C15 H152 . . 109.5 no
C14 C15 H153 . . 109.5 no
H151 C15 H152 . . 109.5 no
H151 C15 H153 . . 109.5 no
H152 C15 H153 . . 109.5 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
Cu1 O1 . 1.949(3) yes
Cu1 O2 . 2.268(4) yes
Cu1 O3 . 1.994(3) yes
Cu1 O4 . 1.951(3) yes
Cu1 N1 . 2.024(4) yes
Cu1 N2 3 2.617(4) yes
O1 C1 . 1.267(5) no
O2 C3 . 1.216(6) no
O3 C6 . 1.242(6) no
O4 C8 . 1.255(6) no
C1 C2 . 1.370(6) no
C1 C4 . 1.532(6) no
C2 C3 . 1.406(7) no
C3 C5 . 1.539(7) no
C6 C7 . 1.398(7) no
C6 C9 . 1.517(8) no
C7 C8 . 1.370(7) no
C8 C10 . 1.522(7) no
N1 C11 . 1.328(5) no
N1 C12 . 1.339(6) no
N2 Cu1 8_454 2.617(4) no
N2 C11 . 1.325(5) no
N2 C14 . 1.347(6) no
C12 C13 . 1.358(7) no
C13 C14 . 1.382(7) no
C14 C15 . 1.475(7) no
C4 F1 . 1.308(6) no
C4 F2 . 1.303(7) no
C4 F3 . 1.314(6) no
C5 F4 . 1.315(8) no
C5 F5 . 1.285(8) no
C5 F6 . 1.298(8) no
C9 F7 . 1.291(10) no
C9 F8 . 1.293(8) no
C9 F9 . 1.292(9) no
C10 F10 . 1.254(7) no
C10 F12 . 1.314(7) no
C10 F11 . 1.352(8) no
C2 H2 . .85(6) no
C7 H7 . .84(5) no
C11 H11 . .9300 no
C12 H12 . .9300 no
C13 H13 . .9300 no
C15 H151 . .9600 no
C15 H151 . .9600 no
C15 H151 . .9600 no
