#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:31:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179332 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/29/4322921.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_4322921
loop_
_publ_author_name
'Cristina Tejel'
'B. Eva Villarroya'
'Miguel A. Ciriano'
'Andrew J. Edwards'
'Fernando J. Lahoz'
'Luis A. Oro'
'Maurizio Lanfranchi'
'Antonio Tiripicchio'
'Marisa Tiripicchio-Camellini'
_publ_contact_author
;
   Dr. Fernando J. Lahoz
   Departamento de Quimica Inorganica - I. C. M. A.
   Facultad de Ciencias
   Universidad de Zaragoza - C.S.I.C.
   50009 Zaragoza, Spain
;
_publ_contact_author_email       LAHOZ@POSTA.UNIZAR.ES
_publ_section_title
;
 Hydrogen Bonding and Isomerism Arising from the Coordination Modes of
 Bridging Benzimidazole-2-thiolate Ligands in Tetranuclear Rhodium
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3954
_journal_page_last               3963
_journal_paper_doi               10.1021/ic971376p
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         'C22 H10 Cl2 N4 O8 Rh4 S2, CH2Cl2'
_chemical_formula_structural
'(\m3-HN2SC7H4)2[{Rh(CO)2}{RhCl(CO)2)}]2 . CH2Cl2'
_chemical_formula_sum            'C23 H12 Cl4 N4 O8 Rh4 S2'
_chemical_formula_weight         1089.93
_chemical_name_systematic
;
bis((mu|3$-benziimidazole-2-thiolato-S,S,N)-(dicarbonyl-rhodium(i))-
(chloride-dicarbonyl-rhodium(i))) dichloromethane solvate
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   21.389(3)
_cell_length_b                   21.389(3)
_cell_length_c                   29.359(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      10
_cell_volume                     13431(4)
_computing_cell_refinement       'DIF4 (Stoe)'
_computing_data_collection       'DIF4 (Stoe)'
_computing_data_reduction        'REDU4 (Stoe)'
_computing_molecular_graphics    'SHELXTL v5 (Siemens, 1994)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens-Stoe AED2 diffractometer'
_diffrn_measurement_method       'ω/2θ scans'
_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  0.0657
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            6242
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.69
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.424
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.156
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needles
_exptl_crystal_F_000             8352
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.430
_refine_diff_density_min         -1.532
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.062
_refine_ls_goodness_of_fit_obs   1.073
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         5897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_restrained_S_obs      1.073
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_obs          0.0463
_refine_ls_shift/esd_max         -0.026
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0843P)²+52.1123P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1253
_refine_ls_wR_factor_obs         0.1179
_reflns_number_observed          5197
_reflns_number_total             5901
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971376p_3.cif
_cod_data_source_block           comp7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0843P)^2^+52.1123P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0843P)^2^+52.1123P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        13431.4(38)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4322921
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Rh1 Rh 0.07902(2) 0.27579(2) 0.016060(15) 0.02367(14) Uani 1 d . .
Rh2 Rh 0.17049(2) 0.32029(2) -0.08362(2) 0.02433(14) Uani 1 d . .
Rh3 Rh 0.18613(2) 0.22442(2) -0.15657(2) 0.02626(14) Uani 1 d . .
Rh4 Rh 0.08451(2) 0.24633(2) -0.25946(2) 0.02745(14) Uani 1 d . .
Cl1 Cl 0.04351(7) 0.37676(7) -0.00255(6) 0.0356(4) Uani 1 d . .
Cl2 Cl 0.08843(8) 0.13930(7) -0.24189(6) 0.0402(4) Uani 1 d . .
S1 S 0.08393(7) 0.25903(6) -0.17909(5) 0.0247(3) Uani 1 d . .
S2 S 0.08290(6) 0.25634(6) -0.06371(5) 0.0236(3) Uani 1 d . .
N1 N 0.0322(2) 0.3758(2) -0.1781(2) 0.0277(11) Uani 1 d . .
H1 H 0.0094(26) 0.3662(25) -0.1976(20) 0.008(14) Uiso 1 d . .
N2 N 0.1087(2) 0.3640(2) -0.1284(2) 0.0256(10) Uani 1 d . .
N3 N 0.0842(3) 0.1291(2) -0.0546(2) 0.0306(12) Uani 1 d . .
H3 H 0.0560(35) 0.1293(35) -0.0406(25) 0.035(22) Uiso 1 d . .
N4 N 0.1423(2) 0.1637(2) -0.1110(2) 0.0261(10) Uani 1 d . .
C1 C 0.0765(3) 0.3370(2) -0.1620(2) 0.0233(12) Uani 1 d . .
C2 C 0.1050(3) 0.1799(3) -0.0771(2) 0.0230(11) Uani 1 d . .
C11 C 0.0350(3) 0.4308(3) -0.1542(2) 0.0298(13) Uani 1 d . .
C12 C -0.0017(3) 0.4855(3) -0.1566(2) 0.0340(14) Uani 1 d . .
H12 H -0.0348(3) 0.4904(3) -0.1778(2) 0.041 Uiso 1 calc R .
C13 C 0.0145(3) 0.5317(3) -0.1255(3) 0.042(2) Uani 1 d . .
H13 H -0.0087(3) 0.5696(3) -0.1254(3) 0.051 Uiso 1 calc R .
C14 C 0.0633(4) 0.5246(3) -0.0943(3) 0.043(2) Uani 1 d . .
H14 H 0.0727(4) 0.5580(3) -0.0741(3) 0.051 Uiso 1 calc R .
C15 C 0.0983(3) 0.4707(3) -0.0920(2) 0.0346(14) Uani 1 d . .
H15 H 0.1310(3) 0.4659(3) -0.0705(2) 0.041 Uiso 1 calc R .
C16 C 0.0834(3) 0.4234(3) -0.1228(2) 0.0273(12) Uani 1 d . .
C21 C 0.1095(3) 0.0759(3) -0.0745(2) 0.0304(13) Uani 1 d . .
C22 C 0.1060(3) 0.0133(3) -0.0629(3) 0.042(2) Uani 1 d . .
H22 H 0.0818(3) -0.0009(3) -0.0378(3) 0.050 Uiso 1 calc R .
C23 C 0.1394(3) -0.0268(3) -0.0899(3) 0.044(2) Uani 1 d . .
H23 H 0.1383(3) -0.0703(3) -0.0834(3) 0.053 Uiso 1 calc R .
C24 C 0.1753(4) -0.0057(3) -0.1269(3) 0.054(2) Uani 1 d . .
H24 H 0.1975(4) -0.0353(3) -0.1448(3) 0.065 Uiso 1 calc R .
C25 C 0.1790(3) 0.0563(3) -0.1378(3) 0.039(2) Uani 1 d . .
H25 H 0.2031(3) 0.0706(3) -0.1629(3) 0.047 Uiso 1 calc R .
C26 C 0.1455(3) 0.0979(3) -0.1099(2) 0.0304(13) Uani 1 d . .
C101 C 0.0736(3) 0.3014(3) 0.0766(2) 0.0333(14) Uani 1 d . .
O101 O 0.0695(2) 0.3187(2) 0.1129(2) 0.0442(12) Uani 1 d . .
C102 C 0.1136(3) 0.2007(3) 0.0338(2) 0.0320(14) Uani 1 d . .
O102 O 0.1366(2) 0.1563(2) 0.0464(2) 0.0432(12) Uani 1 d . .
C201 C 0.2220(3) 0.2794(3) -0.0419(2) 0.0368(15) Uani 1 d . .
O201 O 0.2537(2) 0.2536(3) -0.0175(2) 0.060(2) Uani 1 d . .
C202 C 0.2352(3) 0.3757(3) -0.0987(3) 0.041(2) Uani 1 d . .
O202 O 0.2748(3) 0.4079(3) -0.1081(2) 0.066(2) Uani 1 d . .
C301 C 0.2642(3) 0.1908(3) -0.1409(3) 0.044(2) Uani 1 d . .
O301 O 0.3111(3) 0.1711(3) -0.1319(3) 0.070(2) Uani 1 d . .
C302 C 0.2233(3) 0.2797(3) -0.1972(3) 0.039(2) Uani 1 d . .
O302 O 0.2462(3) 0.3140(2) -0.2211(2) 0.0547(14) Uani 1 d . .
C401 C 0.0882(4) 0.2244(3) -0.3210(2) 0.044(2) Uani 1 d . .
O401 O 0.0919(4) 0.2091(3) -0.3575(2) 0.075(2) Uani 1 d . .
C402 C 0.0841(3) 0.3300(3) -0.2747(2) 0.038(2) Uani 1 d . .
O402 O 0.0858(3) 0.3810(2) -0.2858(2) 0.0554(14) Uani 1 d . .
C500 C 0.2792(5) 0.4664(5) -0.2174(4) 0.076(3) Uani 1 d . .
H50A H 0.2941(5) 0.4809(5) -0.1873(4) 0.091 Uiso 0.50 calc PR 1
H50B H 0.2975(5) 0.4248(5) -0.2237(4) 0.091 Uiso 0.50 calc PR 1
H50C H 0.2952(5) 0.4231(5) -0.2151(4) 0.091 Uiso 0.50 calc PR 2
H50D H 0.2734(5) 0.4823(5) -0.1860(4) 0.091 Uiso 0.50 calc PR 2
Cl3 Cl 0.3002(6) 0.5183(5) -0.2587(3) 0.119(4) Uani 0.50 d P 1
Cl3A Cl 0.3375(4) 0.5142(4) -0.2458(4) 0.086(3) Uani 0.50 d P 2
Cl4 Cl 0.1912(5) 0.4618(4) -0.2180(3) 0.102(3) Uani 0.50 d P 1
Cl4A Cl 0.2117(5) 0.4648(5) -0.2425(4) 0.118(3) Uani 0.50 d P 2
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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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'
Cl Cl 0.1484 0.1585 '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
C102 Rh1 C101 90.6(3) . . ?
C102 Rh1 Cl1 174.0(2) . . ?
C101 Rh1 Cl1 86.1(2) . . ?
C102 Rh1 S2 96.4(2) . . ?
C101 Rh1 S2 172.8(2) . . ?
Cl1 Rh1 S2 86.75(5) . . ?
C201 Rh2 C202 90.9(3) . . ?
C201 Rh2 N2 176.9(2) . . ?
C202 Rh2 N2 92.1(2) . . ?
C201 Rh2 S2 91.9(2) . . ?
C202 Rh2 S2 175.7(2) . . ?
N2 Rh2 S2 85.06(13) . . ?
C201 Rh2 Rh3 94.8(2) . . ?
C202 Rh2 Rh3 100.5(2) . . ?
N2 Rh2 Rh3 85.75(13) . . ?
S2 Rh2 Rh3 82.55(4) . . ?
C302 Rh3 C301 91.2(3) . . ?
C302 Rh3 N4 178.5(2) . . ?
C301 Rh3 N4 90.2(3) . . ?
C302 Rh3 S1 91.0(2) . . ?
C301 Rh3 S1 175.3(2) . . ?
N4 Rh3 S1 87.67(14) . . ?
C302 Rh3 Rh2 94.1(2) . . ?
C301 Rh3 Rh2 100.7(3) . . ?
N4 Rh3 Rh2 85.25(13) . . ?
S1 Rh3 Rh2 83.32(4) . . ?
C402 Rh4 C401 90.6(3) . . ?
C402 Rh4 Cl2 177.8(2) . . ?
C401 Rh4 Cl2 88.0(2) . . ?
C402 Rh4 S1 97.4(2) . . ?
C401 Rh4 S1 171.7(2) . . ?
Cl2 Rh4 S1 83.88(6) . . ?
C1 S1 Rh4 113.2(2) . . ?
C1 S1 Rh3 107.3(2) . . ?
Rh4 S1 Rh3 103.50(6) . . ?
C2 S2 Rh1 113.2(2) . . ?
C2 S2 Rh2 105.6(2) . . ?
Rh1 S2 Rh2 99.66(5) . . ?
H1 N1 C1 122.3(41) . . ?
H1 N1 C11 129.0(41) . . ?
C1 N1 C11 108.6(5) . . ?
C1 N2 C16 106.4(5) . . ?
C1 N2 Rh2 126.8(4) . . ?
C16 N2 Rh2 125.5(4) . . ?
H3 N3 C2 123.1(60) . . ?
H3 N3 C21 124.3(60) . . ?
C2 N3 C21 108.9(5) . . ?
C2 N4 C26 105.9(5) . . ?
C2 N4 Rh3 126.2(4) . . ?
C26 N4 Rh3 127.8(4) . . ?
N2 C1 N1 110.8(5) . . ?
N2 C1 S1 125.3(4) . . ?
N1 C1 S1 123.5(4) . . ?
N4 C2 N3 111.0(5) . . ?
N4 C2 S2 125.3(4) . . ?
N3 C2 S2 123.7(4) . . ?
N1 C11 C16 105.9(5) . . ?
N1 C11 C12 131.5(6) . . ?
C16 C11 C12 122.6(6) . . ?
C13 C12 C11 114.8(6) . . ?
C12 C13 C14 122.7(6) . . ?
C15 C14 C13 121.8(6) . . ?
C14 C15 C16 117.0(6) . . ?
C15 C16 C11 121.1(6) . . ?
C15 C16 N2 130.7(6) . . ?
C11 C16 N2 108.2(5) . . ?
C26 C21 C22 123.2(6) . . ?
C26 C21 N3 104.8(5) . . ?
C22 C21 N3 131.9(6) . . ?
C23 C22 C21 115.9(7) . . ?
C22 C23 C24 122.0(6) . . ?
C25 C24 C23 121.7(7) . . ?
C24 C25 C26 116.6(7) . . ?
C21 C26 C25 120.5(6) . . ?
C21 C26 N4 109.3(5) . . ?
C25 C26 N4 130.2(6) . . ?
O101 C101 Rh1 177.7(6) . . ?
O102 C102 Rh1 176.3(5) . . ?
O201 C201 Rh2 178.2(7) . . ?
O202 C202 Rh2 178.6(7) . . ?
O301 C301 Rh3 179.2(7) . . ?
O302 C302 Rh3 178.5(6) . . ?
O401 C401 Rh4 177.1(7) . . ?
O402 C402 Rh4 176.6(6) . . ?
Cl4A C500 Cl3A 114.5(8) . . ?
Cl3 C500 Cl4 107.0(8) . . ?
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
Rh1 C102 1.843(7) . ?
Rh1 C101 1.862(7) . ?
Rh1 Cl1 2.354(2) . ?
Rh1 S2 2.380(2) . ?
Rh2 C201 1.866(7) . ?
Rh2 C202 1.875(7) . ?
Rh2 N2 2.086(5) . ?
Rh2 S2 2.3923(14) . ?
Rh2 Rh3 2.9839(7) . ?
Rh3 C302 1.859(7) . ?
Rh3 C301 1.875(7) . ?
Rh3 N4 2.088(5) . ?
Rh3 S1 2.4006(15) . ?
Rh4 C402 1.844(7) . ?
Rh4 C401 1.868(7) . ?
Rh4 Cl2 2.348(2) . ?
Rh4 S1 2.375(2) . ?
S1 C1 1.748(5) . ?
S2 C2 1.748(6) . ?
N1 H1 0.78(6) . ?
N1 C1 1.346(8) . ?
N1 C11 1.370(8) . ?
N2 C1 1.333(7) . ?
N2 C16 1.392(7) . ?
N3 H3 0.73(7) . ?
N3 C2 1.346(8) . ?
N3 C21 1.391(8) . ?
N4 C2 1.322(7) . ?
N4 C26 1.408(7) . ?
C11 C16 1.395(9) . ?
C11 C12 1.411(8) . ?
C12 C13 1.389(10) . ?
C13 C14 1.397(11) . ?
C14 C15 1.377(9) . ?
C15 C16 1.392(9) . ?
C21 C26 1.378(9) . ?
C21 C22 1.383(9) . ?
C22 C23 1.370(11) . ?
C23 C24 1.403(12) . ?
C24 C25 1.368(10) . ?
C25 C26 1.405(9) . ?
C101 O101 1.132(8) . ?
C102 O102 1.134(8) . ?
C201 O201 1.129(8) . ?
C202 O202 1.127(8) . ?
C301 O301 1.121(8) . ?
C302 O302 1.127(8) . ?
C401 O401 1.123(9) . ?
C402 O402 1.140(8) . ?
C500 Cl4A 1.621(14) . ?
C500 Cl3 1.705(13) . ?
C500 Cl3A 1.814(14) . ?
C500 Cl4 1.885(15) . ?
