#------------------------------------------------------------------------------
#$Date: 2016-03-22 10:33:38 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178875 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/04/4110444.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_4110444
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)2 (O2 C C (CH3)3)2'
_chemical_formula_sum            'C14 H18 Bi F6 O8 Rh'
_chemical_formula_weight         740.17
_chemical_name_systematic
; 
 bis(mu2-trifluoroacetateo-O,O')-bis(mu2-pivolate-O,O')-(bismuth-rhodium) 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.2932(9)
_cell_length_b                   9.5539(5)
_cell_length_c                   24.9971(12)
_cell_measurement_reflns_used    7747
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.54
_cell_volume                     4368.8(4)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_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  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            36000
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.63
_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    8.887
_exptl_absorpt_correction_T_max  0.6649
_exptl_absorpt_correction_T_min  0.2695
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.251
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.399
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0209P)²+6.3793P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0437
_refine_ls_wR_factor_ref         0.0447
_reflns_number_gt                4786
_reflns_number_total             5235
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja058294hsi20051206_043702.cif
_cod_data_source_block           (1)_BiRh(O2CCF3)2(O2CCMe3)2
_cod_database_code               4110444
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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
Bi1 Bi 0.150053(5) 0.947178(10) 0.142532(4) 0.01517(4) Uani 1 1 d
Rh1 Rh 0.182607(11) 0.69636(2) 0.120164(9) 0.01421(5) Uani 1 1 d
O1 O 0.03652(11) 0.8588(2) 0.15479(9) 0.0233(4) Uani 1 1 d
O2 O 0.11998(12) 0.95533(19) 0.05379(8) 0.0215(4) Uani 1 1 d
O3 O 0.28476(11) 0.96359(19) 0.10029(8) 0.0190(4) Uani 1 1 d
O4 O 0.16370(12) 0.8349(2) 0.23278(8) 0.0242(4) Uani 1 1 d
O5 O 0.08084(11) 0.6421(2) 0.14247(8) 0.0198(4) Uani 1 1 d
O6 O 0.15531(10) 0.7315(2) 0.04361(8) 0.0193(4) Uani 1 1 d
O7 O 0.28772(10) 0.72902(19) 0.09714(8) 0.0176(4) Uani 1 1 d
O8 O 0.21432(11) 0.6426(2) 0.19571(8) 0.0193(4) Uani 1 1 d
C1 C 0.03067(15) 0.7267(3) 0.15548(12) 0.0199(6) Uani 1 1 d
C2 C -0.04279(16) 0.6631(3) 0.17183(13) 0.0242(6) Uani 1 1 d
C3 C 0.13405(14) 0.8488(3) 0.02546(12) 0.0188(6) Uani 1 1 d
C4 C 0.12960(17) 0.8623(3) -0.03503(12) 0.0241(6) Uani 1 1 d
C5 C 0.31353(14) 0.8491(3) 0.08973(11) 0.0159(5) Uani 1 1 d
C6 C 0.38983(16) 0.8439(3) 0.06372(13) 0.0233(6) Uani 1 1 d
F1 F 0.43605(10) 0.7761(2) 0.09570(10) 0.0446(5) Uani 1 1 d
F2 F 0.41732(11) 0.96787(18) 0.05294(9) 0.0339(5) Uani 1 1 d
F3 F 0.38674(12) 0.7728(2) 0.01791(8) 0.0415(5) Uani 1 1 d
C7 C 0.19336(15) 0.7188(3) 0.23389(12) 0.0211(6) Uani 1 1 d
C8 C 0.20345(18) 0.6552(3) 0.28993(12) 0.0269(6) Uani 1 1 d
F4 F 0.13836(12) 0.6126(3) 0.30832(8) 0.0435(5) Uani 1 1 d
F5 F 0.24812(14) 0.5464(2) 0.29054(8) 0.0444(6) Uani 1 1 d
F6 F 0.22906(11) 0.7490(2) 0.32439(7) 0.0360(4) Uani 1 1 d
C9 C -0.0324(3) 0.5121(5) 0.1903(3) 0.0566(13) Uani 1 1 d
C10 C -0.0762(2) 0.7494(6) 0.2166(2) 0.0502(11) Uani 1 1 d
C11 C -0.0912(2) 0.6658(7) 0.12216(19) 0.0520(12) Uani 1 1 d
C12 C 0.2015(2) 0.9303(5) -0.05118(16) 0.0420(9) Uani 1 1 d
C13 C 0.0667(2) 0.9550(4) -0.05094(15) 0.0321(8) Uani 1 1 d
C14 C 0.1220(2) 0.7205(4) -0.06102(14) 0.0297(7) Uani 1 1 d
H9A H -0.002(4) 0.533(7) 0.224(3) 0.12(3) Uiso 1 1 d
H9B H -0.080(3) 0.482(5) 0.2011(18) 0.053(12) Uiso 1 1 d
H9C H -0.019(3) 0.462(5) 0.156(2) 0.055(14) Uiso 1 1 d
H10A H -0.089(3) 0.830(6) 0.199(2) 0.077(19) Uiso 1 1 d
H10B H -0.126(3) 0.705(4) 0.2262(17) 0.051(12) Uiso 1 1 d
H10C H -0.043(3) 0.754(6) 0.243(2) 0.071(16) Uiso 1 1 d
H11A H -0.099(3) 0.762(6) 0.119(2) 0.064(16) Uiso 1 1 d
H11B H -0.143(3) 0.630(5) 0.1301(18) 0.053(13) Uiso 1 1 d
H11C H -0.070(3) 0.629(6) 0.091(2) 0.073(16) Uiso 1 1 d
H12A H 0.199(3) 0.945(4) -0.089(2) 0.055(13) Uiso 1 1 d
H12B H 0.208(3) 1.025(5) -0.0326(18) 0.059(14) Uiso 1 1 d
H12C H 0.241(3) 0.861(5) -0.0439(17) 0.059(13) Uiso 1 1 d
H13A H 0.076(3) 1.035(5) -0.035(2) 0.059(14) Uiso 1 1 d
H13B H 0.069(3) 0.968(5) -0.085(2) 0.055(14) Uiso 1 1 d
H13C H 0.024(2) 0.910(4) -0.0402(15) 0.034(10) Uiso 1 1 d
H14A H 0.164(2) 0.663(5) -0.0545(18) 0.051(13) Uiso 1 1 d
H14B H 0.081(2) 0.690(4) -0.0482(15) 0.030(10) Uiso 1 1 d
H14C H 0.120(2) 0.730(4) -0.0984(16) 0.035(10) 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
O1 Bi1 O2 85.60(8) . . y
O1 Bi1 O4 79.06(7) . . y
O2 Bi1 O4 155.53(7) . . y
O1 Bi1 Rh1 83.83(5) . . y
O2 Bi1 Rh1 82.80(5) . . y
O4 Bi1 Rh1 76.74(5) . . y
O1 Bi1 O3 156.52(7) . . y
O2 Bi1 O3 80.64(7) . . y
O4 Bi1 O3 106.68(7) . . y
Rh1 Bi1 O3 75.67(4) . . y
O6 Rh1 O5 94.43(8) . . y
O6 Rh1 O7 86.54(8) . . y
O5 Rh1 O7 173.90(8) . . y
O6 Rh1 O8 174.51(8) . . y
O5 Rh1 O8 86.66(8) . . y
O7 Rh1 O8 91.82(8) . . y
O6 Rh1 O3 91.14(7) . 8_655 y
O5 Rh1 O3 92.85(7) . 8_655 y
O7 Rh1 O3 81.10(7) . 8_655 y
O8 Rh1 O3 83.43(7) . 8_655 y
O6 Rh1 Bi1 89.64(6) . . y
O5 Rh1 Bi1 87.99(6) . . y
O7 Rh1 Bi1 98.04(5) . . y
O8 Rh1 Bi1 95.78(5) . . y
O3 Rh1 Bi1 178.80(5) 8_655 . y
C1 O1 Bi1 116.83(18) . . ?
C3 O2 Bi1 117.79(18) . . ?
C5 O3 Rh1 140.25(18) . 8_665 ?
C5 O3 Bi1 114.89(16) . . ?
Rh1 O3 Bi1 101.81(7) 8_665 . ?
C7 O4 Bi1 116.59(19) . . ?
C1 O5 Rh1 125.32(18) . . ?
C3 O6 Rh1 124.38(18) . . ?
C5 O7 Rh1 122.60(17) . . ?
C7 O8 Rh1 117.97(18) . . ?
O5 C1 O1 124.8(3) . . ?
O5 C1 C2 116.9(2) . . ?
O1 C1 C2 118.3(3) . . ?
C10 C2 C11 111.0(4) . . ?
C10 C2 C9 109.9(4) . . ?
C11 C2 C9 109.5(4) . . ?
C10 C2 C1 109.5(3) . . ?
C11 C2 C1 106.6(3) . . ?
C9 C2 C1 110.3(3) . . ?
O2 C3 O6 124.9(3) . . ?
O2 C3 C4 118.5(3) . . ?
O6 C3 C4 116.5(3) . . ?
C13 C4 C14 110.1(3) . . ?
C13 C4 C3 110.7(3) . . ?
C14 C4 C3 110.9(3) . . ?
C13 C4 C12 109.9(3) . . ?
C14 C4 C12 110.4(3) . . ?
C3 C4 C12 104.7(3) . . ?
O3 C5 O7 127.9(3) . . ?
O3 C5 C6 120.1(2) . . ?
O7 C5 C6 112.0(2) . . ?
F2 C6 F1 108.6(3) . . ?
F2 C6 F3 107.4(2) . . ?
F1 C6 F3 107.2(2) . . ?
F2 C6 C5 113.8(2) . . ?
F1 C6 C5 109.7(2) . . ?
F3 C6 C5 109.9(2) . . ?
O4 C7 O8 129.4(3) . . ?
O4 C7 C8 115.3(3) . . ?
O8 C7 C8 115.2(2) . . ?
F5 C8 F6 107.7(3) . . ?
F5 C8 F4 107.9(3) . . ?
F6 C8 F4 107.2(3) . . ?
F5 C8 C7 113.3(3) . . ?
F6 C8 C7 111.5(2) . . ?
F4 C8 C7 109.0(3) . . ?
C2 C9 H9A 97(4) . . ?
C2 C9 H9B 105(3) . . ?
H9A C9 H9B 109(5) . . ?
C2 C9 H9C 102(3) . . ?
H9A C9 H9C 131(5) . . ?
H9B C9 H9C 109(4) . . ?
C2 C10 H10A 101(3) . . ?
C2 C10 H10B 108(2) . . ?
H10A C10 H10B 103(4) . . ?
C2 C10 H10C 107(3) . . ?
H10A C10 H10C 119(5) . . ?
H10B C10 H10C 116(4) . . ?
C2 C11 H11A 101(3) . . ?
C2 C11 H11B 112(3) . . ?
H11A C11 H11B 102(4) . . ?
C2 C11 H11C 115(3) . . ?
H11A C11 H11C 111(5) . . ?
H11B C11 H11C 114(4) . . ?
C4 C12 H12A 107(3) . . ?
C4 C12 H12B 111(3) . . ?
H12A C12 H12B 109(4) . . ?
C4 C12 H12C 107(3) . . ?
H12A C12 H12C 108(4) . . ?
H12B C12 H12C 114(4) . . ?
C4 C13 H13A 105(3) . . ?
C4 C13 H13B 109(3) . . ?
H13A C13 H13B 108(4) . . ?
C4 C13 H13C 107(2) . . ?
H13A C13 H13C 116(4) . . ?
H13B C13 H13C 113(4) . . ?
C4 C14 H14A 112(3) . . ?
C4 C14 H14B 103(2) . . ?
H14A C14 H14B 116(3) . . ?
C4 C14 H14C 110(2) . . ?
H14A C14 H14C 105(3) . . ?
H14B C14 H14C 112(3) . . ?
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 O1 2.263(2) . y
Bi1 O2 2.287(2) . y
Bi1 O4 2.510(2) . y
Bi1 Rh1 2.5317(2) . y
Bi1 O3 2.6855(19) . y
Rh1 O6 2.006(2) . y
Rh1 O5 2.011(2) . y
Rh1 O7 2.0313(19) . y
Rh1 O8 2.041(2) . y
Rh1 O3 2.3556(18) 8_655 y
O1 C1 1.267(3) . ?
O2 C3 1.266(3) . ?
O3 C5 1.243(3) . ?
O3 Rh1 2.3556(18) 8_665 ?
O4 C7 1.236(3) . ?
O5 C1 1.265(3) . ?
O6 C3 1.270(3) . ?
O7 C5 1.254(3) . ?
O8 C7 1.260(3) . ?
C1 C2 1.530(4) . ?
C2 C10 1.519(5) . ?
C2 C11 1.525(5) . ?
C2 C9 1.526(5) . ?
C3 C4 1.520(4) . ?
C4 C13 1.506(5) . ?
C4 C14 1.509(4) . ?
C4 C12 1.521(5) . ?
C5 C6 1.540(4) . ?
C6 F2 1.315(3) . ?
C6 F1 1.332(4) . ?
C6 F3 1.332(4) . ?
C7 C8 1.538(4) . ?
C8 F5 1.322(4) . ?
C8 F6 1.329(4) . ?
C8 F4 1.340(4) . ?
C9 H9A 1.04(7) . ?
C9 H9B 0.96(5) . ?
C9 H9C 1.02(5) . ?
C10 H10A 0.92(5) . ?
C10 H10B 1.03(5) . ?
C10 H10C 0.90(5) . ?
C11 H11A 0.93(5) . ?
C11 H11B 1.02(5) . ?
C11 H11C 0.93(5) . ?
C12 H12A 0.96(5) . ?
C12 H12B 1.02(5) . ?
C12 H12C 1.00(5) . ?
C13 H13A 0.87(5) . ?
C13 H13B 0.85(5) . ?
C13 H13C 0.93(4) . ?
C14 H14A 0.96(4) . ?
C14 H14B 0.86(4) . ?
C14 H14C 0.94(4) . ?
