#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:08:53 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178637 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/48/4074854.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_4074854
loop_
_publ_author_name
'Crossley, Ian R.'
'Hill, Anthony F.'
'Humphrey, Elizabeth R.'
'Smith, Matthew K.'
_publ_section_title
;
 A Less Carbocentric View of Agostic Interactions:  The Complexes
 [Rh(η4-cod){H2A(mt)2}] (A = B, C+; mt = Methimazolyl)
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2242
_journal_paper_doi               10.1021/om050942i
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C55 H62 B2 Cl2 F8 N12 Rh2 S4'
_chemical_formula_weight         1452.02
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 106.448(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   17.146(5)
_cell_length_b                   22.332(5)
_cell_length_c                   17.492(5)
_cell_measurement_reflns_used    51448
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     6424(3)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'X -Seed'
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       ' φ and ω scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            57231
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.94
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2950
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.944
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         7379
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0461
_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)+(0.0705P)²+10.0712P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1336
_reflns_number_gt                5523
_reflns_number_total             7379
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050942isi20051102_090428.cif
_cod_data_source_block           c:lh1m
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4074854
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'
'-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
_atom_site_refinement_flags
Rh1 Rh 0.565238(15) 0.088910(12) 0.198815(14) 0.03566(11) Uani 1 1 d .
Cl1 Cl 0.3716(2) 0.47222(11) 0.2676(2) 0.0982(9) Uani 0.50 1 d PDU
F1 F 0.9057(2) 0.14255(18) 0.0885(3) 0.1436(19) Uani 1 1 d .
B1 B 0.8852(3) 0.0940(2) 0.0427(3) 0.0573(12) Uani 1 1 d .
F2 F 0.80979(16) 0.10039(13) -0.0089(2) 0.0862(9) Uani 1 1 d .
C2 C 0.4717(10) 0.4700(8) 0.2801(10) 0.213(12) Uani 0.50 1 d PDU
F3 F 0.8784(3) 0.04745(18) 0.0923(2) 0.1259(13) Uani 1 1 d .
F4 F 0.94111(17) 0.07868(15) 0.00600(18) 0.0879(9) Uani 1 1 d .
S11 S 0.67247(5) 0.05593(4) 0.31155(5) 0.0463(2) Uani 1 1 d .
N11 N 0.83058(18) 0.08519(14) 0.36960(19) 0.0477(7) Uani 1 1 d .
C11 C 0.7624(2) 0.08595(15) 0.3073(2) 0.0398(8) Uani 1 1 d .
N12 N 0.78427(17) 0.11200(13) 0.24609(18) 0.0422(7) Uani 1 1 d .
C12 C 0.8373(3) 0.0590(2) 0.4479(2) 0.0623(11) Uani 1 1 d .
H12A H 0.8113 0.0856 0.4780 0.094 Uiso 1 1 calc R
H12B H 0.8948 0.0540 0.4770 0.094 Uiso 1 1 calc R
H12C H 0.8102 0.0199 0.4410 0.094 Uiso 1 1 calc R
C13 C 0.8942(2) 0.1116(2) 0.3468(3) 0.0609(11) Uani 1 1 d .
H13 H 0.9482 0.1170 0.3799 0.073 Uiso 1 1 calc R
C14 C 0.8666(2) 0.12803(19) 0.2709(3) 0.0543(10) Uani 1 1 d .
H14 H 0.8967 0.1469 0.2396 0.065 Uiso 1 1 calc R
C15 C 0.7339(2) 0.11935(15) 0.1648(2) 0.0388(7) Uani 1 1 d .
H15A H 0.6832 0.0960 0.1571 0.047 Uiso 1 1 calc R
H15B H 0.7631 0.1035 0.1277 0.047 Uiso 1 1 calc R
S21 S 0.59924(6) 0.19206(4) 0.23065(6) 0.0468(2) Uani 1 1 d .
C21 C 0.6583(2) 0.21420(16) 0.17243(19) 0.0408(8) Uani 1 1 d .
N22 N 0.66218(19) 0.27063(13) 0.14489(18) 0.0460(7) Uani 1 1 d .
C22 C 0.6143(3) 0.32160(18) 0.1603(3) 0.0589(11) Uani 1 1 d .
H22A H 0.5670 0.3067 0.1754 0.088 Uiso 1 1 calc R
H22B H 0.5959 0.3460 0.1120 0.088 Uiso 1 1 calc R
H22C H 0.6481 0.3460 0.2037 0.088 Uiso 1 1 calc R
N23 N 0.71359(17) 0.18197(12) 0.14628(16) 0.0392(6) Uani 1 1 d .
C23 C 0.7189(2) 0.27338(17) 0.1027(2) 0.0499(9) Uani 1 1 d .
H23 H 0.7327 0.3078 0.0774 0.050 Uiso 1 1 calc R
C24 C 0.7511(2) 0.21842(17) 0.1040(2) 0.0455(8) Uani 1 1 d .
H24 H 0.7921 0.2069 0.0801 0.055 Uiso 1 1 calc R
N31 N 0.52619(17) -0.04328(14) 0.15787(17) 0.0409(6) Uani 1 1 d .
C31 C 0.53945(19) 0.00698(17) 0.17296(19) 0.0379(7) Uani 1 1 d .
C32 C 0.5205(2) -0.10549(16) 0.1499(2) 0.0404(8) Uani 1 1 d .
C33 C 0.4546(2) -0.12943(18) 0.0918(2) 0.0468(8) Uani 1 1 d .
C34 C 0.3925(3) -0.0899(2) 0.0376(3) 0.0583(11) Uani 1 1 d .
H34A H 0.4158 -0.0717 -0.0020 0.087 Uiso 1 1 calc R
H34B H 0.3763 -0.0583 0.0689 0.087 Uiso 1 1 calc R
H34C H 0.3448 -0.1137 0.0103 0.087 Uiso 1 1 calc R
C35 C 0.4504(3) -0.19196(19) 0.0868(3) 0.0582(11) Uani 1 1 d .
H35 H 0.4066 -0.2105 0.0483 0.070 Uiso 1 1 calc R
C36 C 0.5095(3) -0.22698(19) 0.1375(3) 0.0642(12) Uani 1 1 d .
H36 H 0.5053 -0.2694 0.1337 0.077 Uiso 1 1 calc R
C37 C 0.5732(3) -0.20188(19) 0.1926(3) 0.0579(11) Uani 1 1 d .
H37 H 0.6130 -0.2271 0.2264 0.069 Uiso 1 1 calc R
C38 C 0.5816(2) -0.14010(18) 0.2006(2) 0.0477(9) Uani 1 1 d .
C39 C 0.6519(3) -0.1116(2) 0.2602(3) 0.0587(10) Uani 1 1 d .
H39A H 0.6883 -0.1428 0.2899 0.088 Uiso 1 1 calc R
H39B H 0.6319 -0.0872 0.2972 0.088 Uiso 1 1 calc R
H39C H 0.6817 -0.0861 0.2325 0.088 Uiso 1 1 calc R
N41 N 0.43189(18) 0.13378(15) 0.05459(18) 0.0488(8) Uani 1 1 d .
C41 C 0.4811(2) 0.11588(16) 0.1093(2) 0.0410(8) Uani 1 1 d .
C42 C 0.3673(2) 0.15851(19) -0.0059(2) 0.0489(9) Uani 1 1 d .
C43 C 0.3120(2) 0.1195(2) -0.0548(2) 0.0536(10) Uani 1 1 d .
C44 C 0.3219(3) 0.0526(2) -0.0460(3) 0.0660(12) Uani 1 1 d .
H44A H 0.3705 0.0402 -0.0608 0.099 Uiso 1 1 calc R
H44B H 0.2740 0.0328 -0.0810 0.099 Uiso 1 1 calc R
H44C H 0.3277 0.0413 0.0094 0.099 Uiso 1 1 calc R
C45 C 0.2474(3) 0.1452(2) -0.1123(2) 0.0650(12) Uani 1 1 d .
H45 H 0.2074 0.1202 -0.1462 0.078 Uiso 1 1 calc R
C46 C 0.2409(3) 0.2069(3) -0.1206(3) 0.0708(14) Uani 1 1 d .
H46 H 0.1966 0.2236 -0.1604 0.085 Uiso 1 1 calc R
C47 C 0.2972(3) 0.2440(2) -0.0723(3) 0.0676(12) Uani 1 1 d .
H47 H 0.2917 0.2861 -0.0793 0.081 Uiso 1 1 calc R
C48 C 0.3625(3) 0.2207(2) -0.0128(2) 0.0581(10) Uani 1 1 d .
C49 C 0.4242(3) 0.2607(2) 0.0405(3) 0.0738(13) Uani 1 1 d .
H49A H 0.4280 0.2516 0.0963 0.111 Uiso 1 1 calc R
H49B H 0.4080 0.3025 0.0291 0.111 Uiso 1 1 calc R
H49C H 0.4773 0.2541 0.0312 0.111 Uiso 1 1 calc R
Cl2 Cl 0.4787(3) 0.4186(2) 0.2283(10) 0.170(6) Uani 0.25 1 d PDU
H2B H 0.4975(9) 0.4669(16) 0.3406(11) 0.050 Uiso 0.50 1 d PD
H2A H 0.4890(12) 0.5114(7) 0.267(2) 0.050 Uiso 0.50 1 d PD
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.150
-3 2 0 0.088
-5 -6 0 0.098
3 4 0 0.138
2 -1 -1 0.118
2 -1 -4 0.183
-5 3 4 0.125
1 4 -5 0.181
0 -1 0 0.161
3 -2 0 0.111
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
C41 Rh1 C31 92.16(14) . .
C41 Rh1 S11 179.24(11) . .
C31 Rh1 S11 88.44(10) . .
C41 Rh1 S21 87.99(11) . .
C31 Rh1 S21 179.23(10) . .
S11 Rh1 S21 91.41(4) . .
C2 Cl1 Cl2 36.6(5) . .
F1 B1 F4 113.2(4) . .
F1 B1 F2 110.6(4) . .
F4 B1 F2 112.6(4) . .
F1 B1 F3 106.8(5) . .
F4 B1 F3 107.9(4) . .
F2 B1 F3 105.2(4) . .
Cl2 C2 Cl2 35.2(11) 2_655 .
Cl2 C2 C2 57.4(8) 2_655 2_655
Cl2 C2 C2 55.8(9) . 2_655
Cl2 C2 Cl1 128.1(10) 2_655 .
Cl2 C2 Cl1 101.5(8) . .
C2 C2 Cl1 134.2(16) 2_655 .
C11 S11 Rh1 109.64(12) . .
C11 N11 C13 109.4(3) . .
C11 N11 C12 125.4(3) . .
C13 N11 C12 125.2(3) . .
N11 C11 N12 105.7(3) . .
N11 C11 S11 123.1(3) . .
N12 C11 S11 131.1(3) . .
C11 N12 C14 110.1(3) . .
C11 N12 C15 126.9(3) . .
C14 N12 C15 122.9(3) . .
C14 C13 N11 108.4(3) . .
C13 C14 N12 106.4(3) . .
N12 C15 N23 111.5(3) . .
C21 S21 Rh1 106.65(12) . .
N22 C21 N23 105.1(3) . .
N22 C21 S21 125.5(3) . .
N23 C21 S21 129.3(3) . .
C21 N22 C23 110.1(3) . .
C21 N22 C22 124.5(3) . .
C23 N22 C22 125.3(3) . .
C21 N23 C24 110.0(3) . .
C21 N23 C15 125.1(3) . .
C24 N23 C15 124.7(3) . .
C24 C23 N22 107.4(3) . .
C23 C24 N23 107.3(3) . .
C31 N31 C32 171.2(3) . .
N31 C31 Rh1 178.0(3) . .
C33 C32 N31 118.3(3) . .
C33 C32 C38 123.9(3) . .
N31 C32 C38 117.9(3) . .
C32 C33 C35 116.4(4) . .
C32 C33 C34 121.3(4) . .
C35 C33 C34 122.3(4) . .
C36 C35 C33 120.5(4) . .
C37 C36 C35 121.2(4) . .
C36 C37 C38 121.4(4) . .
C37 C38 C32 116.6(4) . .
C37 C38 C39 122.2(4) . .
C32 C38 C39 121.3(4) . .
C41 N41 C42 173.4(4) . .
N41 C41 Rh1 177.7(3) . .
C43 C42 C48 123.8(4) . .
C43 C42 N41 118.1(4) . .
C48 C42 N41 118.1(4) . .
C45 C43 C42 116.9(4) . .
C45 C43 C44 121.8(4) . .
C42 C43 C44 121.4(3) . .
C46 C45 C43 120.6(4) . .
C47 C46 C45 121.0(4) . .
C46 C47 C48 120.8(5) . .
C42 C48 C47 116.8(4) . .
C42 C48 C49 121.8(4) . .
C47 C48 C49 121.4(4) . .
Cl2 Cl2 C2 74.1(7) 2_655 2_655
Cl2 Cl2 C2 70.7(14) 2_655 .
C2 Cl2 C2 66.7(14) 2_655 .
Cl2 Cl2 Cl1 105.1(18) 2_655 .
C2 Cl2 Cl1 98.5(7) 2_655 .
C2 Cl2 Cl1 41.9(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 C41 1.902(4) .
Rh1 C31 1.906(4) .
Rh1 S11 2.3996(10) .
Rh1 S21 2.4026(11) .
Cl1 C2 1.668(17) .
Cl1 Cl2 2.448(10) .
F1 B1 1.334(6) .
B1 F4 1.340(6) .
B1 F2 1.359(6) .
B1 F3 1.381(6) .
C2 Cl2 1.462(19) 2_655
C2 Cl2 1.489(16) .
C2 C2 1.62(4) 2_655
S11 C11 1.702(4) .
N11 C11 1.354(4) .
N11 C13 1.394(5) .
N11 C12 1.463(5) .
C11 N12 1.361(5) .
N12 C14 1.400(5) .
N12 C15 1.448(4) .
C13 C14 1.329(6) .
C15 N23 1.455(4) .
S21 C21 1.700(4) .
C21 N22 1.358(4) .
C21 N23 1.368(4) .
N22 C23 1.379(5) .
N22 C22 1.472(5) .
N23 C24 1.376(4) .
C23 C24 1.343(5) .
N31 C31 1.161(4) .
N31 C32 1.397(5) .
C32 C33 1.394(5) .
C32 C38 1.399(5) .
C33 C35 1.400(6) .
C33 C34 1.498(6) .
C35 C36 1.384(6) .
C36 C37 1.357(6) .
C37 C38 1.390(6) .
C38 C39 1.494(5) .
N41 C41 1.153(4) .
N41 C42 1.409(5) .
C42 C43 1.390(6) .
C42 C48 1.394(6) .
C43 C45 1.391(6) .
C43 C44 1.506(7) .
C45 C46 1.386(7) .
C46 C47 1.368(7) .
C47 C48 1.395(6) .
C48 C49 1.493(7) .
Cl2 Cl2 0.89(3) 2_655
Cl2 C2 1.462(19) 2_655
