#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/78/4327871.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_4327871
loop_
_publ_author_name
'Alexander S. Filatov'
'Margaret Napier'
'Volodimir D. Vreshch'
'Natalie J. Sumner'
'Evgeny V. Dikarev'
'Marina A. Petrukhina'
_publ_contact_author_address
;
Department of Chemistry
University at Albany
1400 Washington ave
Albany NY 12222
USA
;
_publ_contact_author_email       marina@albany.edu
_publ_contact_author_fax         518-442-3462
_publ_contact_author_name
;
 Dikarev, Evgeny V.
;
_publ_contact_author_phone       518-442-4406
_publ_section_title
;
 From Solid State to Solution: Advancing Chemistry of Bi-Bi and Bi-Rh
 Paddlewheel Carboxylates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              566
_journal_page_last               571
_journal_paper_doi               10.1021/ic202089p
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C8 Bi F12 O8 Rh'
_chemical_formula_sum            'C8 Bi F12 O8 Rh'
_chemical_formula_weight         763.97
_chemical_name_systematic
; 
 tetrakis(μ₂-trifluoroacetato-O,O')-bismuth-rhodium(II,II) 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   none
_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            4
_cell_length_a                   9.7707(5)
_cell_length_b                   12.3992(7)
_cell_length_c                   13.0323(7)
_cell_measurement_reflns_used    9678
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.76
_cell_volume                     1578.85(15)
_computing_cell_refinement       'SAINT Ver. 6.22  (Bruker-AXS, 2003)'
_computing_data_collection       'SMART Ver. 5.622 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT Ver. 6.22'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'
_computing_structure_refinement  'SHELXTL Ver. 6.14'
_computing_structure_solution    'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '0.30° ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12221
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    12.353
_exptl_absorpt_correction_T_max  0.3714
_exptl_absorpt_correction_T_min  0.1914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2003)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.214
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.207
_refine_diff_density_min         -1.327
_refine_diff_density_rms         0.183
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.009(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3585
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0264
_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)+(0.0201P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0567
_reflns_number_gt                3126
_reflns_number_total             3585
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic202089p_si_002_3.cif
_cod_data_source_block           2
_cod_original_sg_symbol_Hall     'P 2c -2n    '
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_database_code               4327871
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, 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 0.15065(2) 0.617496(17) 0.73490(4) 0.01956(7) Uani 1 1 d
Rh1 Rh 0.39994(5) 0.64083(4) 0.67943(4) 0.01893(11) Uani 1 1 d
O1 O 0.4396(4) 0.4876(3) 0.7270(6) 0.0253(10) Uani 1 1 d
O2 O 0.2238(5) 0.4436(4) 0.7657(4) 0.0320(16) Uani 1 1 d
O3 O 0.3546(5) 0.5872(4) 0.5367(4) 0.0252(12) Uani 1 1 d
O4 O 0.1332(5) 0.5514(5) 0.5671(5) 0.0352(14) Uani 1 1 d
O5 O 0.3754(5) 0.7936(4) 0.6307(4) 0.0228(11) Uani 1 1 d
O6 O 0.1456(5) 0.8024(4) 0.6483(4) 0.0250(12) Uani 1 1 d
O7 O 0.4617(5) 0.6987(4) 0.8173(4) 0.0237(11) Uani 1 1 d
O8 O 0.2647(5) 0.6601(4) 0.8967(4) 0.0291(12) Uani 1 1 d
C1 C 0.3482(7) 0.4258(6) 0.7567(5) 0.0226(19) Uani 1 1 d
C2 C 0.3932(8) 0.3107(6) 0.7876(7) 0.0294(18) Uani 1 1 d
C3 C 0.2384(8) 0.5562(6) 0.5135(6) 0.0233(16) Uani 1 1 d
C4 C 0.2213(8) 0.5164(7) 0.4008(7) 0.0280(18) Uani 1 1 d
C5 C 0.2572(7) 0.8386(6) 0.6224(6) 0.0203(15) Uani 1 1 d
C6 C 0.2663(8) 0.9527(7) 0.5754(7) 0.0272(19) Uani 1 1 d
C7 C 0.3830(7) 0.6929(6) 0.8935(6) 0.0220(16) Uani 1 1 d
C8 C 0.4450(9) 0.7340(7) 0.9944(6) 0.0292(18) Uani 1 1 d
F1 F 0.3724(8) 0.2958(5) 0.8851(5) 0.086(3) Uani 1 1 d
F2 F 0.3227(5) 0.2393(3) 0.7361(7) 0.0647(16) Uani 1 1 d
F3 F 0.5205(5) 0.2908(4) 0.7679(5) 0.059(2) Uani 1 1 d
F4 F 0.0971(5) 0.5353(5) 0.3658(4) 0.0398(13) Uani 1 1 d
F5 F 0.2396(6) 0.4076(4) 0.3974(4) 0.0434(14) Uani 1 1 d
F6 F 0.3113(5) 0.5592(5) 0.3391(4) 0.0451(13) Uani 1 1 d
F7 F 0.3368(5) 0.9506(4) 0.4884(4) 0.0381(12) Uani 1 1 d
F8 F 0.1451(5) 0.9916(5) 0.5558(6) 0.064(2) Uani 1 1 d
F9 F 0.3328(6) 1.0182(4) 0.6386(5) 0.0574(17) Uani 1 1 d
F10 F 0.3519(5) 0.7450(4) 1.0672(4) 0.0402(13) Uani 1 1 d
F11 F 0.5063(5) 0.8293(4) 0.9824(4) 0.0388(12) Uani 1 1 d
F12 F 0.5403(5) 0.6645(4) 1.0281(4) 0.0416(12) Uani 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'
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'
Bi Bi -4.1077 10.2566 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O2 Bi1 O4 81.8(2)
O2 Bi1 O8 84.89(19)
O4 Bi1 O8 156.23(18)
O2 Bi1 O6 157.11(17)
O4 Bi1 O6 84.2(2)
O8 Bi1 O6 101.31(18)
O2 Bi1 Rh1 81.94(12)
O4 Bi1 Rh1 81.07(13)
O8 Bi1 Rh1 77.59(12)
O6 Bi1 Rh1 78.01(10)
O5 Rh1 O3 89.6(2)
O5 Rh1 O7 89.0(2)
O3 Rh1 O7 174.9(2)
O5 Rh1 O1 175.83(19)
O3 Rh1 O1 90.9(3)
O7 Rh1 O1 90.2(2)
O5 Rh1 Bi1 94.72(13)
O3 Rh1 Bi1 90.82(14)
O7 Rh1 Bi1 94.18(14)
O1 Rh1 Bi1 89.41(14)
C1 O1 Rh1 122.4(4)
C1 O2 Bi1 117.0(5)
C3 O3 Rh1 121.8(5)
C3 O4 Bi1 116.6(5)
C5 O5 Rh1 122.8(4)
C5 O6 Bi1 115.6(4)
C7 O7 Rh1 119.9(5)
C7 O8 Bi1 118.2(5)
O1 C1 O2 128.7(7)
O1 C1 C2 116.6(6)
O2 C1 C2 114.7(6)
F3 C2 F1 108.5(7)
F3 C2 F2 105.9(7)
F1 C2 F2 108.8(8)
F3 C2 C1 113.5(7)
F1 C2 C1 110.0(7)
F2 C2 C1 110.0(6)
O3 C3 O4 129.5(8)
O3 C3 C4 115.3(7)
O4 C3 C4 115.2(7)
F6 C4 F4 109.6(7)
F6 C4 F5 107.1(7)
F4 C4 F5 106.6(7)
F6 C4 C3 112.3(7)
F4 C4 C3 111.7(6)
F5 C4 C3 109.2(7)
O6 C5 O5 128.0(7)
O6 C5 C6 119.7(6)
O5 C5 C6 112.3(6)
F8 C6 F9 109.8(8)
F8 C6 F7 108.1(7)
F9 C6 F7 106.8(7)
F8 C6 C5 111.4(7)
F9 C6 C5 110.1(7)
F7 C6 C5 110.5(7)
O8 C7 O7 128.5(7)
O8 C7 C8 116.9(7)
O7 C7 C8 114.6(6)
F10 C8 F11 107.5(7)
F10 C8 F12 108.0(7)
F11 C8 F12 107.2(7)
F10 C8 C7 112.2(7)
F11 C8 C7 111.8(7)
F12 C8 C7 110.0(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Bi1 O2 2.307(5)
Bi1 O4 2.342(6)
Bi1 O8 2.443(5)
Bi1 O6 2.556(5)
Bi1 Rh1 2.5571(6)
Rh1 O5 2.012(5)
Rh1 O3 2.024(5)
Rh1 O7 2.027(5)
Rh1 O1 2.035(5)
O1 C1 1.239(9)
O2 C1 1.241(8)
O3 C3 1.236(8)
O4 C3 1.244(9)
O5 C5 1.288(8)
O6 C5 1.227(8)
O7 C7 1.258(9)
O8 C7 1.226(8)
C1 C2 1.546(10)
C2 F3 1.294(9)
C2 F1 1.300(10)
C2 F2 1.307(10)
C3 C4 1.559(11)
C4 F6 1.304(9)
C4 F4 1.318(9)
C4 F5 1.362(9)
C5 C6 1.544(11)
C6 F8 1.304(9)
C6 F9 1.327(10)
C6 F7 1.328(9)
C7 C8 1.534(11)
C8 F10 1.321(9)
C8 F11 1.335(9)
C8 F12 1.343(9)
