#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/55/7035573.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_7035573
loop_
_publ_author_name
'Zhu, Di'
'Sharma, Arzoo Z.'
'Wiebe, Christopher R.'
'Budzelaar, Peter H. M.'
_publ_section_title
;
 Rhodium(ii) dimers without metal-metal bonds.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13460
_journal_page_last               13463
_journal_paper_doi               10.1039/c5dt02218e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C42 H62 I2 N4 Rh2, C7'
_chemical_formula_sum            'C49 H62 I2 N4 Rh2'
_chemical_formula_weight         1166.65
_chemical_name_systematic
'{bis(μ₂-Iodo)-bis(N,N'-bis(2,6-dimethylphenyl)pentane-2,4-diiminato-N,N')-diphenyl-di-rhodium(II) toluene solvate'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-06-09 deposited with the CCDC.
2015-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 131.886(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.268(7)
_cell_length_b                   11.773(4)
_cell_length_c                   14.410(4)
_cell_measurement_reflns_used    9848
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.095
_cell_measurement_theta_min      2.840
_cell_volume                     2433.5(14)
_computing_cell_refinement       'APEX2 software suite'
_computing_data_collection       'APEX2 software suite'
_computing_data_reduction        'APEX2 software suite'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker D8 three-circle diffractometer with an APEX-II CCD detector'
_diffrn_measurement_method       'area detector φ and ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0122
_diffrn_reflns_av_sigmaI/netI    0.0112
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9067
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.84
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    1.982
_exptl_absorpt_correction_T_max  0.9805
_exptl_absorpt_correction_T_min  0.8094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'a irregular fragment'
_exptl_crystal_F_000             1160
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, hexane, THF'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.00062(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2396
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0577P)²+3.7955P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                2256
_reflns_number_total             2396
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c5dt02218e3.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7035573--7035574.cif.'
_cod_original_cell_volume        2433.4(14)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7035573
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
'-x, -y, -z'
'-x, y, -z'
'-x+1/2, -y+1/2, -z'
'-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
_atom_site_refinement_flags
Rh1 Rh 0.08292(2) 0.5000 0.45998(3) 0.03848(14) Uani 1 2 d S
I1 I -0.095636(19) 0.5000 0.34555(3) 0.06044(16) Uani 1 2 d S
C11 C 0.3704(3) 0.5000 0.6115(5) 0.0693(14) Uani 1 2 d S
H111 H 0.3913 0.5305 0.5721 0.104 Uiso 1 1 calc R
H112 H 0.3929 0.4236 0.6383 0.104 Uiso 1 1 calc R
H113 H 0.3939 0.5458 0.6824 0.104 Uiso 1 1 calc R
C12 C 0.2654(3) 0.5000 0.5203(4) 0.0491(10) Uani 1 2 d S
C13 C 0.2199(4) 0.5000 0.3954(5) 0.0564(12) Uani 1 2 d S
H13 H 0.2582 0.5000 0.3775 0.068 Uiso 1 2 calc SR
C14 C 0.1255(3) 0.5000 0.2934(4) 0.0483(10) Uani 1 2 d S
C15 C 0.0952(4) 0.5000 0.1667(4) 0.0643(13) Uani 1 2 d S
H151 H 0.1457 0.5257 0.1734 0.096 Uiso 1 1 calc R
H152 H 0.0428 0.5499 0.1125 0.096 Uiso 1 1 calc R
H153 H 0.0778 0.4244 0.1332 0.096 Uiso 1 1 calc R
N1 N 0.2208(2) 0.5000 0.5613(3) 0.0420(8) Uani 1 2 d S
N2 N 0.0613(3) 0.5000 0.3030(3) 0.0452(8) Uani 1 2 d S
C21 C 0.2798(3) 0.5000 0.6958(4) 0.0481(10) Uani 1 2 d S
C22 C 0.3060(2) 0.3964(4) 0.7577(4) 0.0690(10) Uani 1 1 d .
C23 C 0.3621(3) 0.4003(7) 0.8872(4) 0.106(2) Uani 1 1 d .
H23 H 0.3814 0.3328 0.9317 0.127 Uiso 1 1 calc R
C24 C 0.3888(6) 0.5000 0.9488(7) 0.133(5) Uani 1 2 d S
H24 H 0.4260 0.5000 1.0349 0.160 Uiso 1 2 calc SR
C27 C 0.2744(4) 0.2869(4) 0.6881(6) 0.0990(17) Uani 1 1 d .
H271 H 0.2078 0.2878 0.6219 0.148 Uiso 1 1 calc R
H272 H 0.2921 0.2253 0.7439 0.148 Uiso 1 1 calc R
H273 H 0.3029 0.2770 0.6538 0.148 Uiso 1 1 calc R
C31 C -0.0351(3) 0.5000 0.1863(4) 0.0550(12) Uani 1 2 d S
C32 C -0.0795(3) 0.6043(4) 0.1342(3) 0.0736(11) Uani 1 1 d .
C33 C -0.1739(3) 0.6011(7) 0.0241(4) 0.111(2) Uani 1 1 d .
H33 H -0.2058 0.6688 -0.0141 0.134 Uiso 1 1 calc R
C34 C -0.2199(5) 0.5000 -0.0280(7) 0.125(4) Uani 1 2 d S
H34 H -0.2829 0.5000 -0.0995 0.150 Uiso 1 2 calc SR
C37 C -0.0307(4) 0.7140(4) 0.1933(5) 0.0929(15) Uani 1 1 d .
H371 H 0.0020 0.7114 0.2806 0.139 Uiso 1 1 calc R
H372 H -0.0754 0.7746 0.1547 0.139 Uiso 1 1 calc R
H373 H 0.0130 0.7269 0.1829 0.139 Uiso 1 1 calc R
C91 C 0.0000 0.1719(12) 0.5000 0.159(4) Uiso 1 2 d SD
C92 C 0.0692(8) 0.0998(7) 0.6028(10) 0.108(3) Uiso 0.50 1 d PD
C93 C 0.0736(5) -0.0209(6) 0.6098(7) 0.080(2) Uiso 0.50 1 d PD
C94 C 0.0000 -0.0733(12) 0.5000 0.088(4) Uiso 0.50 2 d SPD
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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
N1 Rh1 N2 89.85(15) . .
N1 Rh1 I1 174.83(10) . .
N2 Rh1 I1 95.33(11) . .
N1 Rh1 I1 95.07(10) . 5_566
N2 Rh1 I1 175.08(11) . 5_566
I1 Rh1 I1 79.756(19) . 5_566
Rh1 I1 Rh1 100.24(2) . 5_566
C12 C11 H111 109.5 . .
C12 C11 H112 109.5 . .
H111 C11 H112 109.5 . .
C12 C11 H113 109.5 . .
H111 C11 H113 109.5 . .
H112 C11 H113 109.5 . .
N1 C12 C13 123.0(4) . .
N1 C12 C11 120.1(4) . .
C13 C12 C11 116.9(4) . .
C12 C13 C14 128.8(4) . .
C12 C13 H13 115.6 . .
C14 C13 H13 115.6 . .
N2 C14 C13 123.0(4) . .
N2 C14 C15 119.5(4) . .
C13 C14 C15 117.4(4) . .
C14 C15 H151 109.5 . .
C14 C15 H152 109.5 . .
H151 C15 H152 109.5 . .
C14 C15 H153 109.5 . .
H151 C15 H153 109.5 . .
H152 C15 H153 109.5 . .
C12 N1 C21 115.6(4) . .
C12 N1 Rh1 127.8(3) . .
C21 N1 Rh1 116.6(3) . .
C14 N2 C31 116.0(4) . .
C14 N2 Rh1 127.5(3) . .
C31 N2 Rh1 116.5(3) . .
C22 C21 C22 122.5(5) . 2_565
C22 C21 N1 118.8(2) . .
C22 C21 N1 118.8(2) 2_565 .
C21 C22 C23 116.8(5) . .
C21 C22 C27 121.1(4) . .
C23 C22 C27 122.0(5) . .
C24 C23 C22 121.5(6) . .
C24 C23 H23 119.3 . .
C22 C23 H23 119.3 . .
C23 C24 C23 120.9(7) . 2_565
C23 C24 H24 119.6 . .
C23 C24 H24 119.6 2_565 .
C22 C27 H271 109.5 . .
C22 C27 H272 109.5 . .
H271 C27 H272 109.5 . .
C22 C27 H273 109.5 . .
H271 C27 H273 109.5 . .
H272 C27 H273 109.5 . .
C32 C31 C32 123.4(5) 2_565 .
C32 C31 N2 118.3(3) 2_565 .
C32 C31 N2 118.3(3) . .
C31 C32 C33 116.7(5) . .
C31 C32 C37 122.1(4) . .
C33 C32 C37 121.2(5) . .
C34 C33 C32 121.2(6) . .
C34 C33 H33 119.4 . .
C32 C33 H33 119.4 . .
C33 C34 C33 120.6(7) 2_565 .
C33 C34 H34 119.7 2_565 .
C33 C34 H34 119.7 . .
C32 C37 H371 109.5 . .
C32 C37 H372 109.5 . .
H371 C37 H372 109.5 . .
C32 C37 H373 109.5 . .
H371 C37 H373 109.5 . .
H372 C37 H373 109.5 . .
C94 C91 C92 53.7(6) 5_556 .
C94 C91 C92 53.7(6) 5_556 6_556
C92 C91 C92 107.4(13) . 6_556
C93 C92 C94 79.6(10) 2 5_556
C93 C92 C93 1.6(3) 2 .
C94 C92 C93 78.0(8) 5_556 .
C93 C92 C91 131.0(14) 2 .
C94 C92 C91 51.4(9) 5_556 .
C93 C92 C91 129.4(11) . .
C93 C93 C92 175.3(9) 2 2
C93 C93 C94 116.6(6) 2 .
C92 C93 C94 58.7(8) 2 .
C93 C93 C92 3.1(6) 2 .
C92 C93 C92 172.2(14) 2 .
C94 C93 C92 113.5(10) . .
C93 C93 C94 48.0(5) 2 5_556
C92 C93 C94 127.3(11) 2 5_556
C94 C93 C94 68.6(10) . 5_556
C92 C93 C94 44.9(6) . 5_556
C91 C94 C92 74.9(7) 5_556 2
C91 C94 C92 74.9(7) 5_556 5_556
C92 C94 C92 149.8(14) 2 5_556
C91 C94 C93 116.6(6) 5_556 6_556
C92 C94 C93 168.5(12) 2 6_556
C92 C94 C93 41.7(6) 5_556 6_556
C91 C94 C93 116.6(6) 5_556 .
C92 C94 C93 41.7(6) 2 .
C92 C94 C93 168.5(12) 5_556 .
C93 C94 C93 126.8(12) 6_556 .
C91 C94 C93 132.0(5) 5_556 5_556
C92 C94 C93 153.1(12) 2 5_556
C92 C94 C93 57.1(4) 5_556 5_556
C93 C94 C93 15.4(4) 6_556 5_556
C93 C94 C93 111.4(10) . 5_556
C91 C94 C93 132.0(5) 5_556 2
C92 C94 C93 57.1(4) 2 2
C92 C94 C93 153.1(12) 5_556 2
C93 C94 C93 111.4(10) 6_556 2
C93 C94 C93 15.4(4) . 2
C93 C94 C93 96.0(10) 5_556 2
C91 C94 C94 179.997(1) 5_556 5_556
C92 C94 C94 105.1(7) 2 5_556
C92 C94 C94 105.1(7) 5_556 5_556
C93 C94 C94 63.4(6) 6_556 5_556
C93 C94 C94 63.4(6) . 5_556
C93 C94 C94 48.0(5) 5_556 5_556
C93 C94 C94 48.0(5) 2 5_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 N1 2.003(4) .
Rh1 N2 2.008(4) .
Rh1 I1 2.6420(11) .
Rh1 I1 2.6449(9) 5_566
I1 Rh1 2.6449(9) 5_566
C11 C12 1.507(6) .
C11 H111 0.9600 .
C11 H112 0.9600 .
C11 H113 0.9600 .
C12 N1 1.328(6) .
C12 C13 1.379(7) .
C13 C14 1.379(7) .
C13 H13 0.9300 .
C14 N2 1.332(6) .
C14 C15 1.500(6) .
C15 H151 0.9600 .
C15 H152 0.9600 .
C15 H153 0.9600 .
N1 C21 1.451(5) .
N2 C31 1.452(6) .
C21 C22 1.392(4) .
C21 C22 1.392(4) 2_565
C22 C23 1.399(6) .
C22 C27 1.490(7) .
C23 C24 1.349(7) .
C23 H23 0.9300 .
C24 C23 1.349(7) 2_565
C24 H24 0.9300 .
C27 H271 0.9600 .
C27 H272 0.9600 .
C27 H273 0.9600 .
C31 C32 1.394(5) 2_565
C31 C32 1.394(5) .
C32 C33 1.405(6) .
C32 C37 1.486(7) .
C33 C34 1.370(8) .
C33 H33 0.9300 .
C34 C33 1.370(8) 2_565
C34 H34 0.9300 .
C37 H371 0.9600 .
C37 H372 0.9600 .
C37 H373 0.9600 .
C91 C94 1.161(16) 5_556
C91 C92 1.434(8) .
C91 C92 1.434(8) 6_556
C92 C93 0.931(13) 2
C92 C94 1.197(11) 5_556
C92 C93 1.423(8) .
C93 C93 0.493(15) 2
C93 C92 0.931(13) 2
C93 C94 1.378(7) .
C93 C94 1.658(13) 5_556
C94 C91 1.161(16) 5_556
C94 C92 1.197(11) 2
C94 C92 1.197(11) 5_556
C94 C93 1.378(7) 6_556
C94 C93 1.658(13) 5_556
C94 C93 1.658(13) 2
C94 C94 1.73(3) 5_556
