#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:09:45 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178887 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/16/4111663.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4111663
loop_
_publ_author_name
'Evgeny V. Dikarev'
'Haitao Zhang'
'Bo Li'
_publ_section_title
;
 Heterometallic Bismuth-Transition Metal Homoleptic β-Diketonates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6156
_journal_page_last               6157
_journal_paper_doi               10.1021/ja051265m
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'Bi2 Cu (C F3 C O C H C O C F3)8'
_chemical_formula_sum            'C40 H8 Bi2 Cu F48 O16'
_chemical_formula_weight         2137.96
_chemical_name_systematic
; 
 di(bis(1,1,1,5,5,5-hexafluoroacetylacetonato)-(mu2-1,1,1,5,5,5-hexafluoro-
 acetylacetonato)-bismuth(iii))-bis(1,1,1,5,5,5-hexafluoroacetylacetonato)-
 copper(ii) 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.7220(10)
_cell_angle_beta                 76.4600(10)
_cell_angle_gamma                69.6340(10)
_cell_formula_units_Z            1
_cell_length_a                   8.6959(5)
_cell_length_b                   11.2432(6)
_cell_length_c                   16.8765(9)
_cell_measurement_reflns_used    5566
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.53
_cell_volume                     1467.66(14)
_computing_cell_refinement       'SMART, SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXCIF-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '0.3 deg wide ω exposures'
_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  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12928
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    6.557
_exptl_absorpt_correction_T_max  0.8276
_exptl_absorpt_correction_T_min  0.4201
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    2.419
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             1003
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       na
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         6615
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0260P)²+1.9012P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0516
_reflns_number_gt                6337
_reflns_number_total             6615
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja051265msi20050226_020651.cif
_cod_data_source_block           Bi2Cu(hfac)8_(5)
_cod_database_code               4111663
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.796334(12) 0.917290(9) 0.715910(6) 0.01266(4) Uani 1 1 d . . .
Cu1 Cu 1.0000 1.0000 0.5000 0.01333(10) Uani 1 2 d S . .
O1 O 1.0075(3) 0.71170(19) 0.70767(13) 0.0173(4) Uani 1 1 d . A .
O2 O 0.6862(3) 0.75720(19) 0.80011(13) 0.0174(4) Uani 1 1 d . A .
O3 O 1.0701(2) 0.9436(2) 0.64953(13) 0.0156(4) Uani 1 1 d . . .
O4 O 0.9121(2) 0.8721(2) 0.82562(13) 0.0164(4) Uani 1 1 d . . .
O5 O 0.8190(3) 1.12096(19) 0.72313(13) 0.0169(4) Uani 1 1 d . . .
O6 O 0.5625(3) 1.0080(2) 0.80175(13) 0.0183(4) Uani 1 1 d . . .
O7 O 0.7979(2) 1.10870(19) 0.55105(13) 0.0155(4) Uani 1 1 d . . .
O8 O 0.9010(2) 0.86117(19) 0.54456(13) 0.0159(4) Uani 1 1 d . . .
C2 C 1.0323(4) 0.6080(3) 0.7630(2) 0.0210(6) Uani 1 1 d . . .
C3 C 0.9203(4) 0.5693(3) 0.8305(2) 0.0223(6) Uani 1 1 d . A .
C4 C 0.7541(4) 0.6462(3) 0.84093(19) 0.0203(6) Uani 1 1 d . . .
C5 C 0.6297(4) 0.5932(3) 0.9100(2) 0.0228(6) Uani 1 1 d . A .
C6 C 1.3393(4) 0.9562(4) 0.6308(2) 0.0274(7) Uani 1 1 d . . .
C7 C 1.1853(4) 0.9278(3) 0.6882(2) 0.0191(6) Uani 1 1 d . . .
C8 C 1.1885(4) 0.8894(3) 0.7751(2) 0.0215(6) Uani 1 1 d . . .
C9 C 1.0580(4) 0.8649(3) 0.83428(19) 0.0179(6) Uani 1 1 d . . .
C10 C 1.0762(4) 0.8244(3) 0.9269(2) 0.0236(6) Uani 1 1 d . . .
C11 C 0.8385(4) 1.2842(3) 0.7797(2) 0.0222(6) Uani 1 1 d . . .
C12 C 0.7546(4) 1.1841(3) 0.77966(19) 0.0174(6) Uani 1 1 d . . .
C13 C 0.6172(4) 1.1766(3) 0.83972(19) 0.0202(6) Uani 1 1 d . . .
H13 H 0.5824 1.2304 0.8791 0.024 Uiso 1 1 calc R . .
C14 C 0.5290(4) 1.0927(3) 0.84406(18) 0.0167(6) Uani 1 1 d . . .
C15 C 0.3663(4) 1.0994(3) 0.9054(2) 0.0214(6) Uani 1 1 d . . .
C16 C 0.5927(4) 1.2978(3) 0.58479(19) 0.0181(6) Uani 1 1 d . . .
C17 C 0.7685(4) 1.2290(3) 0.54569(18) 0.0157(5) Uani 1 1 d . . .
C18 C 0.9706(4) 0.7464(3) 0.53445(18) 0.0164(6) Uani 1 1 d . . .
C19 C 1.1281(4) 0.6949(3) 0.4932(2) 0.0190(6) Uani 1 1 d . . .
C20 C 0.8601(4) 0.6562(3) 0.5697(2) 0.0204(6) Uani 1 1 d . . .
C1 C 1.2097(4) 0.5150(3) 0.7498(2) 0.0265(7) Uani 1 1 d D A 1
F1 F 1.3219(6) 0.5763(5) 0.7405(5) 0.0185(11) Uiso 0.40 1 d PD A 1
F2 F 1.2315(6) 0.4707(6) 0.6783(4) 0.0177(10) Uiso 0.40 1 d PD A 1
F3 F 1.2400(7) 0.4101(5) 0.8117(4) 0.0252(11) Uiso 0.40 1 d PD A 1
F1X F 1.3219(10) 0.5777(8) 0.7112(6) 0.037(2) Uiso 0.30 1 d PD A 2
F2X F 1.2262(11) 0.4297(9) 0.7118(7) 0.047(2) Uiso 0.30 1 d PD A 2
F3X F 1.2624(12) 0.4501(10) 0.8271(5) 0.051(2) Uiso 0.30 1 d PD A 2
F1Y F 1.3128(12) 0.5483(11) 0.7746(7) 0.057(3) Uiso 0.30 1 d PD A 3
F2Y F 1.2545(11) 0.5099(9) 0.6679(5) 0.041(2) Uiso 0.30 1 d PD A 3
F3Y F 1.2166(10) 0.3912(7) 0.7853(6) 0.0367(18) Uiso 0.30 1 d PD A 3
F4 F 0.6961(3) 0.4718(2) 0.94921(16) 0.0457(6) Uani 1 1 d . . .
F5 F 0.5037(3) 0.5934(2) 0.87750(14) 0.0360(5) Uani 1 1 d . . .
F6 F 0.5669(3) 0.6665(2) 0.96596(13) 0.0335(5) Uani 1 1 d . . .
F7 F 1.3895(3) 0.8916(4) 0.57143(18) 0.0786(12) Uani 1 1 d . . .
F8 F 1.3023(3) 1.0814(3) 0.5945(2) 0.0742(11) Uani 1 1 d . . .
F9 F 1.4669(2) 0.9278(2) 0.67041(12) 0.0294(4) Uani 1 1 d . . .
F10 F 1.0453(3) 0.7123(2) 0.96115(14) 0.0409(6) Uani 1 1 d . . .
F11 F 0.9688(3) 0.9128(2) 0.96647(13) 0.0352(5) Uani 1 1 d . . .
F12 F 1.2273(2) 0.8121(2) 0.93921(13) 0.0341(5) Uani 1 1 d . . .
F13 F 0.9708(3) 1.2812(2) 0.72192(16) 0.0463(6) Uani 1 1 d . . .
F14 F 0.7342(3) 1.40439(19) 0.76569(16) 0.0385(5) Uani 1 1 d . . .
F15 F 0.8860(3) 1.2625(2) 0.85316(14) 0.0351(5) Uani 1 1 d . . .
F16 F 0.3262(3) 1.1908(2) 0.94883(13) 0.0322(5) Uani 1 1 d . . .
F17 F 0.3786(2) 0.98575(19) 0.95971(12) 0.0285(4) Uani 1 1 d . . .
F18 F 0.2424(2) 1.1232(2) 0.86393(13) 0.0310(4) Uani 1 1 d . . .
F19 F 0.4988(2) 1.36220(19) 0.52497(13) 0.0283(4) Uani 1 1 d . . .
F20 F 0.5951(2) 1.38400(18) 0.62475(12) 0.0256(4) Uani 1 1 d . . .
F21 F 0.5206(2) 1.21444(17) 0.63857(12) 0.0244(4) Uani 1 1 d . . .
F22 F 0.7914(3) 0.6505(2) 0.50858(14) 0.0345(5) Uani 1 1 d . . .
F23 F 0.9467(3) 0.53550(18) 0.60141(14) 0.0324(5) Uani 1 1 d . . .
F24 F 0.7394(2) 0.6978(2) 0.62918(13) 0.0300(5) Uani 1 1 d . . .
H8 H 1.292(4) 0.879(3) 0.794(2) 0.012(8) Uiso 1 1 d . . .
H3 H 0.949(5) 0.481(4) 0.869(2) 0.024(10) Uiso 1 1 d . . .
H19 H 1.161(5) 0.610(4) 0.493(2) 0.022(9) Uiso 1 1 d . . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Bi Bi -4.1077 10.2566 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Bi1 O6 82.89(8) . . y
O4 Bi1 O2 79.56(8) . . y
O6 Bi1 O2 70.35(7) . . y
O4 Bi1 O5 75.39(7) . . y
O6 Bi1 O5 73.89(7) . . y
O2 Bi1 O5 138.32(7) . . y
O4 Bi1 O1 76.58(7) . . y
O6 Bi1 O1 140.65(7) . . y
O2 Bi1 O1 73.12(7) . . y
O5 Bi1 O1 130.40(7) . . y
O4 Bi1 O3 79.89(7) . . y
O6 Bi1 O3 140.82(7) . . y
O2 Bi1 O3 138.79(7) . . y
O5 Bi1 O3 67.82(7) . . y
O1 Bi1 O3 67.56(7) . . y
O7 Cu1 O7 180.00(12) . 2_776 y
O7 Cu1 O8 86.32(8) . . y
O7 Cu1 O8 93.68(8) 2_776 . y
O7 Cu1 O8 93.68(8) . 2_776 y
O7 Cu1 O8 86.32(8) 2_776 2_776 y
O8 Cu1 O8 180.00(13) . 2_776 y
O7 Cu1 O3 81.10(7) . . y
O7 Cu1 O3 98.90(7) 2_776 . y
O8 Cu1 O3 83.30(7) . . y
O8 Cu1 O3 96.70(7) 2_776 . y
C2 O1 Bi1 128.07(19) . . y
C4 O2 Bi1 131.2(2) . . n
C7 O3 Bi1 124.86(19) . . n
C7 O3 Cu1 141.81(19) . . n
Bi1 O3 Cu1 93.33(6) . . n
C9 O4 Bi1 131.97(19) . . n
C12 O5 Bi1 128.88(19) . . n
C14 O6 Bi1 132.86(19) . . n
C17 O7 Cu1 124.17(19) . . n
C18 O8 Cu1 124.20(19) . . n
O1 C2 C3 128.1(3) . . n
O1 C2 C1 113.2(3) . . n
C3 C2 C1 118.6(3) . . n
C2 C3 C4 120.4(3) . . n
C2 C3 H3 122(2) . . n
C4 C3 H3 117(2) . . n
O2 C4 C3 129.1(3) . . n
O2 C4 C5 112.0(3) . . n
C3 C4 C5 119.0(3) . . n
F6 C5 F4 108.5(3) . . n
F6 C5 F5 107.5(3) . . n
F4 C5 F5 106.8(3) . . n
F6 C5 C4 111.0(3) . . n
F4 C5 C4 112.8(3) . . n
F5 C5 C4 110.0(3) . . n
F7 C6 F8 107.2(3) . . n
F7 C6 F9 107.5(3) . . n
F8 C6 F9 107.5(3) . . n
F7 C6 C7 111.3(3) . . n
F8 C6 C7 109.4(3) . . n
F9 C6 C7 113.6(3) . . n
O3 C7 C8 128.6(3) . . n
O3 C7 C6 113.4(3) . . n
C8 C7 C6 118.0(3) . . n
C9 C8 C7 124.6(3) . . n
C9 C8 H8 118(2) . . n
C7 C8 H8 117(2) . . n
O4 C9 C8 130.1(3) . . n
O4 C9 C10 110.2(3) . . n
C8 C9 C10 119.7(3) . . n
F11 C10 F10 108.1(3) . . n
F11 C10 F12 107.7(3) . . n
F10 C10 F12 108.3(3) . . n
F11 C10 C9 109.6(3) . . n
F10 C10 C9 110.3(3) . . n
F12 C10 C9 112.5(3) . . n
F13 C11 F15 107.7(3) . . n
F13 C11 F14 107.6(3) . . n
F15 C11 F14 107.3(3) . . n
F13 C11 C12 112.2(3) . . n
F15 C11 C12 110.9(3) . . n
F14 C11 C12 110.9(3) . . n
O5 C12 C13 128.3(3) . . n
O5 C12 C11 114.9(3) . . n
C13 C12 C11 116.8(3) . . n
C12 C13 C14 121.8(3) . . n
C12 C13 H13 119.1 . . n
C14 C13 H13 119.1 . . n
O6 C14 C13 128.3(3) . . n
O6 C14 C15 112.1(3) . . n
C13 C14 C15 119.6(3) . . n
F16 C15 F18 108.2(3) . . n
F16 C15 F17 107.7(3) . . n
F18 C15 F17 107.7(3) . . n
F16 C15 C14 113.1(3) . . n
F18 C15 C14 109.8(3) . . n
F17 C15 C14 110.1(2) . . n
F21 C16 F19 108.2(2) . . n
F21 C16 F20 108.2(2) . . n
F19 C16 F20 107.6(2) . . n
F21 C16 C17 112.0(2) . . n
F19 C16 C17 109.6(2) . . n
F20 C16 C17 111.1(2) . . n
O7 C17 C19 128.1(3) . 2_776 n
O7 C17 C16 114.7(2) . . n
C19 C17 C16 117.1(3) 2_776 . n
O8 C18 C19 128.2(3) . . n
O8 C18 C20 114.3(3) . . n
C19 C18 C20 117.4(3) . . ?
C17 C19 C18 121.5(3) 2_776 . n
C17 C19 H19 121(2) 2_776 . n
C18 C19 H19 118(2) . . n
F24 C20 F23 107.7(3) . . n
F24 C20 F22 108.2(3) . . n
F23 C20 F22 107.2(2) . . n
F24 C20 C18 112.0(2) . . n
F23 C20 C18 111.9(3) . . n
F22 C20 C18 109.6(3) . . n
F3 C1 F1 108.8(5) . . n
F3 C1 F2 106.5(4) . . n
F1 C1 F2 108.5(5) . . n
F3 C1 C2 113.2(3) . . n
F1 C1 C2 110.8(3) . . n
F2 C1 C2 108.8(3) . . n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Bi1 O4 2.165(2) . y
Bi1 O6 2.298(2) . y
Bi1 O2 2.303(2) . y
Bi1 O5 2.404(2) . y
Bi1 O1 2.417(2) . y
Bi1 O3 2.463(2) . y
Cu1 O7 1.926(2) . y
Cu1 O7 1.926(2) 2_776 y
Cu1 O8 1.928(2) . y
Cu1 O8 1.928(2) 2_776 y
Cu1 O3 2.588(2) . y
O1 C2 1.260(4) . n
O2 C4 1.255(4) . n
O3 C7 1.256(4) . n
O4 C9 1.283(4) . n
O5 C12 1.257(4) . n
O6 C14 1.262(4) . n
O7 C17 1.267(3) . n
O8 C18 1.262(4) . n
C2 C3 1.391(4) . n
C2 C1 1.539(4) . n
C3 C4 1.401(4) . n
C3 H3 1.00(4) . n
C4 C5 1.534(4) . n
C5 F6 1.323(4) . n
C5 F4 1.326(4) . n
C5 F5 1.335(4) . n
C6 F7 1.306(4) . n
C6 F8 1.324(5) . n
C6 F9 1.327(4) . n
C6 C7 1.533(4) . n
C7 C8 1.412(4) . n
C8 C9 1.377(4) . n
C8 H8 0.98(3) . n
C9 C10 1.531(4) . n
C10 F11 1.319(4) . n
C10 F10 1.323(4) . n
C10 F12 1.331(4) . n
C11 F13 1.319(4) . n
C11 F15 1.330(4) . n
C11 F14 1.331(4) . n
C11 C12 1.541(4) . n
C12 C13 1.384(4) . n
C13 C14 1.386(4) . n
C13 H13 0.9500 . n
C14 C15 1.537(4) . n
C15 F16 1.329(4) . n
C15 F18 1.330(4) . n
C15 F17 1.333(4) . n
C16 F21 1.327(3) . n
C16 F19 1.332(4) . n
C16 F20 1.335(3) . n
C16 C17 1.536(4) . n
C17 C19 1.384(4) 2_776 n
C18 C19 1.387(4) . n
C18 C20 1.542(4) . n
C19 C17 1.384(4) 2_776 n
C19 H19 0.89(4) . n
C20 F24 1.325(4) . n
C20 F23 1.328(4) . n
C20 F22 1.333(4) . n
C1 F3 1.332(6) . n
C1 F1 1.337(6) . n
C1 F2 1.380(6) . n
