#------------------------------------------------------------------------------
#$Date: 2016-03-22 10:33:38 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178875 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/04/4110445.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_4110445
loop_
_publ_author_name
'Evgeny V. Dikarev'
'Bo Li'
'Haitao Zhang'
_publ_section_title
;
 Tuning the Properties at Heterobimetallic Core: Mixed-Ligand
 Bismuth-Rhodium Paddlewheel Carboxylates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2814
_journal_page_last               2815
_journal_paper_doi               10.1021/ja058294h
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'Bi Rh (O2 C C F3)3 (O2 C C C H3)1'
_chemical_formula_sum            'C8 H3 Bi F9 O8 Rh'
_chemical_formula_weight         709.99
_chemical_name_systematic
; 
 tris(mu2-trifluoroacetateo-O,O')-(mu2-acetate-O,O')-(bismuth-rhodium) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.1210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7690(6)
_cell_length_b                   19.8500(13)
_cell_length_c                   9.4931(6)
_cell_measurement_reflns_used    5214
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.45
_cell_volume                     1595.20(18)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_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  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13679
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.05
_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    12.188
_exptl_absorpt_correction_T_max  0.5284
_exptl_absorpt_correction_T_min  0.3474
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.956
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.195
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0224
_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)+(0.0299P)²+3.7151P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0561
_reflns_number_gt                3503
_reflns_number_total             3735
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja058294hsi20051206_043716.cif
_cod_data_source_block           (2)_BiRh(O2CCF3)3(O2CCH3)
_cod_database_code               4110445
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Bi1 Bi 0.283347(18) 0.338281(7) 0.534286(15) 0.02190(6) Uani 1 1 d
Rh1 Rh 0.22265(4) 0.313270(15) 0.26292(3) 0.01881(7) Uani 1 1 d
O1 O 0.1852(3) 0.22244(14) 0.5244(3) 0.0237(6) Uani 1 1 d
O2 O 0.0177(4) 0.37826(18) 0.4640(3) 0.0360(7) Uani 1 1 d
O3 O 0.3316(4) 0.44787(15) 0.4425(3) 0.0356(7) Uani 1 1 d
O4 O 0.5374(4) 0.29928(17) 0.5164(3) 0.0315(7) Uani 1 1 d
O5 O 0.1335(3) 0.22145(14) 0.2817(3) 0.0241(6) Uani 1 1 d
O6 O 0.0083(3) 0.35804(15) 0.2278(3) 0.0263(6) Uani 1 1 d
O7 O 0.3069(4) 0.40350(14) 0.2196(3) 0.0266(6) Uani 1 1 d
O8 O 0.4352(3) 0.26879(15) 0.2831(3) 0.0250(6) Uani 1 1 d
C1 C 0.1335(5) 0.1937(2) 0.4009(4) 0.0223(8) Uani 1 1 d
C2 C 0.0682(7) 0.1243(2) 0.3944(5) 0.0329(10) Uani 1 1 d
C3 C 0.5427(5) 0.2719(2) 0.4015(4) 0.0248(8) Uani 1 1 d
C4 C 0.6958(5) 0.2370(2) 0.3963(5) 0.0325(10) Uani 1 1 d
C5 C 0.3304(5) 0.4504(2) 0.3122(5) 0.0255(8) Uani 1 1 d
C6 C 0.3567(6) 0.5194(2) 0.2484(5) 0.0335(10) Uani 1 1 d
C7 C -0.0434(5) 0.3806(2) 0.3301(5) 0.0274(9) Uani 1 1 d
C8 C -0.2006(6) 0.4197(3) 0.2817(5) 0.0372(11) Uani 1 1 d
F1 F -0.1693(5) 0.48512(19) 0.2875(6) 0.0914(16) Uani 1 1 d
F2 F -0.2811(5) 0.4053(3) 0.1513(4) 0.0878(15) Uani 1 1 d
F3 F -0.2907(4) 0.40884(18) 0.3695(4) 0.0556(9) Uani 1 1 d
F4 F 0.4939(4) 0.52258(18) 0.2174(5) 0.0718(12) Uani 1 1 d
F5 F 0.2457(4) 0.53027(16) 0.1261(4) 0.0608(10) Uani 1 1 d
F6 F 0.3488(5) 0.56943(15) 0.3355(4) 0.0664(11) Uani 1 1 d
F7 F 0.6702(5) 0.17258(19) 0.3739(6) 0.0811(13) Uani 1 1 d
F8 F 0.8062(4) 0.2449(3) 0.5199(4) 0.0781(13) Uani 1 1 d
F9 F 0.7542(4) 0.2616(2) 0.2911(4) 0.0654(10) Uani 1 1 d
H2A H 0.137(6) 0.098(3) 0.408(6) 0.028(14) Uiso 1 1 d
H2B H 0.014(5) 0.110(2) 0.287(5) 0.027(12) Uiso 1 1 d
H2C H 0.012(6) 0.113(2) 0.462(5) 0.031(13) 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'
Rh Rh -1.1178 0.9187 '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
O2 Bi1 O4 160.38(10) . . y
O2 Bi1 O3 81.38(12) . . y
O4 Bi1 O3 90.67(12) . . y
O2 Bi1 O1 89.64(11) . . y
O4 Bi1 O1 91.03(10) . . y
O3 Bi1 O1 157.31(10) . . y
O2 Bi1 Rh1 81.39(7) . . y
O4 Bi1 Rh1 79.55(7) . . y
O3 Bi1 Rh1 79.66(7) . . y
O1 Bi1 Rh1 78.41(6) . . y
O5 Rh1 O7 173.52(11) . . y
O5 Rh1 O8 88.06(12) . . y
O7 Rh1 O8 91.67(12) . . y
O5 Rh1 O6 92.68(12) . . y
O7 Rh1 O6 87.16(12) . . y
O8 Rh1 O6 176.07(11) . . ?
O5 Rh1 O1 81.34(10) . 4_565 y
O7 Rh1 O1 92.21(11) . 4_565 y
O8 Rh1 O1 81.44(10) . 4_565 y
O6 Rh1 O1 94.84(11) . 4_565 y
O5 Rh1 Bi1 94.06(8) . . y
O7 Rh1 Bi1 92.42(8) . . y
O8 Rh1 Bi1 92.59(8) . . y
O6 Rh1 Bi1 91.21(8) . . y
O1 Rh1 Bi1 172.55(7) 4_565 . ?
C1 O1 Rh1 133.5(2) . 4_566 ?
C1 O1 Bi1 119.5(2) . . ?
Rh1 O1 Bi1 106.96(10) 4_566 . ?
C7 O2 Bi1 115.3(3) . . ?
C5 O3 Bi1 116.1(3) . . ?
C3 O4 Bi1 117.0(3) . . ?
C1 O5 Rh1 124.6(3) . . ?
C7 O6 Rh1 122.4(3) . . ?
C5 O7 Rh1 121.0(3) . . ?
C3 O8 Rh1 121.1(3) . . ?
O5 C1 O1 123.2(4) . . ?
O5 C1 C2 117.3(4) . . ?
O1 C1 C2 119.5(4) . . ?
O4 C3 O8 128.1(4) . . ?
O4 C3 C4 117.9(4) . . ?
O8 C3 C4 114.0(4) . . ?
F7 C4 F8 108.4(5) . . ?
F7 C4 F9 108.8(4) . . ?
F8 C4 F9 106.6(4) . . ?
F7 C4 C3 109.6(4) . . ?
F8 C4 C3 111.4(4) . . ?
F9 C4 C3 111.9(4) . . ?
O3 C5 O7 128.7(4) . . ?
O3 C5 C6 117.9(4) . . ?
O7 C5 C6 113.4(4) . . ?
F6 C6 F4 108.0(4) . . ?
F6 C6 F5 106.4(4) . . ?
F4 C6 F5 107.6(4) . . ?
F6 C6 C5 112.9(4) . . ?
F4 C6 C5 111.8(4) . . ?
F5 C6 C5 109.8(4) . . ?
O2 C7 O6 129.0(4) . . ?
O2 C7 C8 115.9(4) . . ?
O6 C7 C8 115.1(4) . . ?
F2 C8 F3 107.8(5) . . ?
F2 C8 F1 108.3(5) . . ?
F3 C8 F1 106.7(4) . . ?
F2 C8 C7 113.4(4) . . ?
F3 C8 C7 111.6(4) . . ?
F1 C8 C7 108.7(4) . . ?
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 O2 2.385(3) . y
Bi1 O4 2.406(3) . y
Bi1 O3 2.421(3) . y
Bi1 O1 2.449(3) . y
Bi1 Rh1 2.5398(3) . y
Rh1 O5 2.009(3) . y
Rh1 O7 2.020(3) . y
Rh1 O8 2.026(3) . y
Rh1 O6 2.026(3) . y
Rh1 O1 2.313(3) 4_565 y
O1 C1 1.276(5) . ?
O1 Rh1 2.313(3) 4_566 ?
O2 C7 1.245(5) . ?
O3 C5 1.235(5) . ?
O4 C3 1.231(5) . ?
O5 C1 1.259(5) . ?
O6 C7 1.257(5) . ?
O7 C5 1.260(5) . ?
O8 C3 1.266(5) . ?
C1 C2 1.487(6) . ?
C3 C4 1.523(6) . ?
C4 F7 1.305(6) . ?
C4 F8 1.322(6) . ?
C4 F9 1.328(6) . ?
C5 C6 1.539(6) . ?
C6 F6 1.306(6) . ?
C6 F4 1.312(6) . ?
C6 F5 1.324(6) . ?
C7 C8 1.543(6) . ?
C8 F2 1.287(6) . ?
C8 F3 1.308(6) . ?
C8 F1 1.325(6) . ?
