#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/55/7035574.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_7035574
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 Br2 N4 Rh2, C7'
_chemical_formula_sum            'C49 H62 Br2 N4 Rh2'
_chemical_formula_weight         1072.67
_chemical_name_systematic
'bis(μ₂-Bromo)-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     direct
_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                 131.564(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.862(7)
_cell_length_b                   11.848(5)
_cell_length_c                   14.220(5)
_cell_measurement_reflns_used    9409
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.988
_cell_measurement_theta_min      2.8855
_cell_volume                     2377.7(16)
_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  0.0147
_diffrn_reflns_av_sigmaI/netI    0.0123
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_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            8868
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    2.411
_exptl_absorpt_correction_T_max  0.9805
_exptl_absorpt_correction_T_min  0.7724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            deep-green
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'a irregular block'
_exptl_crystal_F_000             1088
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, hexane, thf'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.031
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0036(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2336
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0347
_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)+(0.0639P)²+5.9921P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                2251
_reflns_number_total             2336
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c5dt02218e3.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 7035573--7035574.cif.'
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7035574
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 0.11750(2) 0.5000 0.03682(3) 0.03854(19) Uani 1 2 d S
Br1 Br 0.05639(3) 0.5000 0.14746(4) 0.0615(2) Uani 1 2 d S
C11 C 0.2543(4) 0.5000 -0.1190(6) 0.0703(17) Uani 1 2 d S
H111 H 0.3140 0.5343 -0.0816 0.106 Uiso 1 1 calc R
H112 H 0.2040 0.5420 -0.1922 0.106 Uiso 1 1 calc R
H113 H 0.2535 0.4237 -0.1425 0.106 Uiso 1 1 calc R
C12 C 0.2409(4) 0.5000 -0.0253(5) 0.0502(11) Uani 1 2 d S
C13 C 0.3229(4) 0.5000 0.1007(5) 0.0599(14) Uani 1 2 d S
H13 H 0.3800 0.5000 0.1183 0.072 Uiso 1 2 calc SR
C14 C 0.3288(3) 0.5000 0.2035(5) 0.0535(12) Uani 1 2 d S
C15 C 0.4263(4) 0.5000 0.3312(5) 0.0677(16) Uani 1 2 d S
H151 H 0.4272 0.5473 0.3867 0.102 Uiso 1 1 calc R
H152 H 0.4708 0.5283 0.3250 0.102 Uiso 1 1 calc R
H153 H 0.4435 0.4244 0.3637 0.102 Uiso 1 1 calc R
N1 N 0.1543(3) 0.5000 -0.0661(4) 0.0410(8) Uani 1 2 d S
N2 N 0.2540(3) 0.5000 0.1938(4) 0.0433(9) Uani 1 2 d S
C21 C 0.0770(4) 0.5000 -0.2003(5) 0.0532(13) Uani 1 2 d S
C22 C 0.0413(3) 0.6030(5) -0.2622(5) 0.0834(16) Uani 1 1 d .
C23 C -0.0327(5) 0.5978(10) -0.3933(6) 0.136(4) Uani 1 1 d .
H23 H -0.0585 0.6647 -0.4387 0.163 Uiso 1 1 calc R
C24 C -0.0669(8) 0.5000 -0.4541(9) 0.181(10) Uani 1 2 d S
H24 H -0.1158 0.5000 -0.5410 0.218 Uiso 1 2 calc SR
C27 C 0.0795(6) 0.7109(5) -0.1930(8) 0.127(3) Uani 1 1 d .
H271 H 0.0687 0.7160 -0.1360 0.191 Uiso 1 1 calc R
H272 H 0.0483 0.7726 -0.2515 0.191 Uiso 1 1 calc R
H273 H 0.1463 0.7144 -0.1465 0.191 Uiso 1 1 calc R
C31 C 0.2727(3) 0.5000 0.3099(4) 0.0520(12) Uani 1 2 d S
C32 C 0.2804(3) 0.3965(5) 0.3629(4) 0.0691(12) Uani 1 1 d .
C33 C 0.2963(4) 0.4013(7) 0.4749(5) 0.099(2) Uani 1 1 d .
H33 H 0.3022 0.3344 0.5137 0.119 Uiso 1 1 calc R
C34 C 0.3031(6) 0.5000 0.5270(7) 0.116(4) Uani 1 2 d S
H34 H 0.3127 0.5000 0.6001 0.139 Uiso 1 2 calc SR
C37 C 0.2708(4) 0.2876(5) 0.3029(5) 0.0955(18) Uani 1 1 d .
H371 H 0.2190 0.2926 0.2138 0.143 Uiso 1 1 calc R
H372 H 0.2591 0.2278 0.3365 0.143 Uiso 1 1 calc R
H373 H 0.3283 0.2724 0.3197 0.143 Uiso 1 1 calc R
C81 C 0.0000 0.1817(19) 0.0000 0.14(2) Uiso 0.50 2 d SPD
C82 C 0.0000 0.0650(12) 0.0000 0.086(4) Uiso 0.50 2 d SPD
C83 C -0.0334(7) 0.0000 -0.1030(8) 0.097(2) Uiso 1 2 d SD
C84 C -0.0349(10) -0.1119(7) -0.1087(13) 0.106(4) Uiso 0.50 1 d PD
C85 C 0.0000 -0.164(3) 0.0000 0.16(3) 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'
Br Br -0.2901 2.4595 '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 90.07(17) . .
N1 Rh1 Br1 174.88(11) . .
N2 Rh1 Br1 95.05(12) . .
N1 Rh1 Br1 94.86(12) . 5_565
N2 Rh1 Br1 175.07(11) . 5_565
Br1 Rh1 Br1 80.02(4) . 5_565
Rh1 Br1 Rh1 99.98(4) . 5_565
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 124.1(5) . .
N1 C12 C11 119.6(5) . .
C13 C12 C11 116.3(5) . .
C12 C13 C14 126.9(5) . .
C12 C13 H13 116.5 . .
C14 C13 H13 116.5 . .
N2 C14 C13 123.6(5) . .
N2 C14 C15 119.5(5) . .
C13 C14 C15 116.8(5) . .
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 116.8(4) . .
C12 N1 Rh1 127.5(3) . .
C21 N1 Rh1 115.6(3) . .
C14 N2 C31 116.5(4) . .
C14 N2 Rh1 127.7(3) . .
C31 N2 Rh1 115.7(3) . .
C22 C21 C22 122.8(6) . 2_565
C22 C21 N1 118.6(3) . .
C22 C21 N1 118.6(3) 2_565 .
C21 C22 C23 116.1(7) . .
C21 C22 C27 121.4(5) . .
C23 C22 C27 122.5(7) . .
C24 C23 C22 121.8(9) . .
C24 C23 H23 119.1 . .
C22 C23 H23 119.1 . .
C23 C24 C23 121.4(9) 2_565 .
C23 C24 H24 119.3 2_565 .
C23 C24 H24 119.3 . .
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 122.9(5) . 2_565
C32 C31 N2 118.5(3) . .
C32 C31 N2 118.5(3) 2_565 .
C31 C32 C33 116.2(5) . .
C31 C32 C37 121.4(4) . .
C33 C32 C37 122.4(5) . .
C34 C33 C32 121.9(6) . .
C34 C33 H33 119.1 . .
C32 C33 H33 119.1 . .
C33 C34 C33 120.9(7) . 2_565
C33 C34 H34 119.5 . .
C33 C34 H34 119.5 2_565 .
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 . .
C85 C81 C82 0.013(7) 5 .
C85 C81 C84 55.7(7) 5 5
C82 C81 C84 55.7(7) . 5
C85 C81 C84 55.7(7) 5 2
C82 C81 C84 55.7(7) . 2
C84 C81 C84 111.5(14) 5 2
C85 C82 C84 65.4(6) 5 5
C85 C82 C84 65.4(6) 5 2
C84 C82 C84 130.8(13) 5 2
C85 C82 C81 0.002(1) 5 .
C84 C82 C81 65.4(6) 5 .
C84 C82 C81 65.4(6) 2 .
C85 C82 C83 123.9(6) 5 .
C84 C82 C83 170.7(12) 5 .
C84 C82 C83 58.4(4) 2 .
C81 C82 C83 123.8(6) . .
C85 C82 C83 123.8(6) 5 5
C84 C82 C83 58.4(4) 5 5
C84 C82 C83 170.7(12) 2 5
C81 C82 C83 123.8(6) . 5
C83 C82 C83 112.3(12) . 5
C85 C82 C82 179.996(1) 5 5
C84 C82 C82 114.6(6) 5 5
C84 C82 C82 114.6(6) 2 5
C81 C82 C82 180.0 . 5
C83 C82 C82 56.2(6) . 5
C83 C82 C82 56.2(6) 5 5
C84 C83 C84 174.3(14) . 2
C84 C83 C82 126.7(11) . .
C84 C83 C82 59.0(7) 2 .
C84 C83 C82 59.0(7) . 5
C84 C83 C82 126.7(11) 2 5
C82 C83 C82 67.7(12) . 5
C83 C84 C82 62.6(6) . 5
C83 C84 C85 114(2) . .
C82 C84 C85 51.7(17) 5 .
C83 C84 C81 121.4(11) . 5
C82 C84 C81 58.9(7) 5 5
C85 C84 C81 7.2(13) . 5
C81 C85 C82 179.984(7) 5 5
C81 C85 C84 117.1(14) 5 .
C82 C85 C84 62.9(14) 5 .
C81 C85 C84 117.1(14) 5 6
C82 C85 C84 62.9(14) 5 6
C84 C85 C84 126(3) . 6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 N1 1.993(4) .
Rh1 N2 1.996(4) .
Rh1 Br1 2.4921(9) .
Rh1 Br1 2.4939(11) 5_565
Br1 Rh1 2.4939(11) 5_565
C11 C12 1.512(7) .
C11 H111 0.9600 .
C11 H112 0.9600 .
C11 H113 0.9600 .
C12 N1 1.321(7) .
C12 C13 1.388(8) .
C13 C14 1.390(8) .
C13 H13 0.9300 .
C14 N2 1.322(7) .
C14 C15 1.500(7) .
C15 H151 0.9600 .
C15 H152 0.9600 .
C15 H153 0.9600 .
N1 C21 1.441(6) .
N2 C31 1.442(6) .
C21 C22 1.390(6) .
C21 C22 1.390(6) 2_565
C22 C23 1.405(8) .
C22 C27 1.478(9) .
C23 C24 1.329(11) .
C23 H23 0.9300 .
C24 C23 1.329(11) 2_565
C24 H24 0.9300 .
C27 H271 0.9600 .
C27 H272 0.9600 .
C27 H273 0.9600 .
C31 C32 1.396(5) .
C31 C32 1.396(5) 2_565
C32 C33 1.412(7) .
C32 C37 1.490(8) .
C33 C34 1.343(8) .
C33 H33 0.9300 .
C34 C33 1.343(8) 2_565
C34 H34 0.9300 .
C37 H371 0.9600 .
C37 H372 0.9600 .
C37 H373 0.9600 .
C81 C85 0.21(4) 5
C81 C82 1.383(16) .
C81 C84 1.469(18) 5
C81 C84 1.469(18) 2
C82 C85 1.18(3) 5
C82 C84 1.335(13) 5
C82 C84 1.335(13) 2
C82 C83 1.382(8) .
C82 C83 1.382(8) 5
C82 C82 1.54(3) 5
C83 C84 1.327(9) .
C83 C84 1.327(9) 2
C83 C82 1.382(8) 5
C84 C82 1.335(13) 5
C84 C85 1.364(9) .
C84 C81 1.469(18) 5
C85 C81 0.21(4) 5
C85 C82 1.18(3) 5
C85 C84 1.364(9) 6
