#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:58:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179402 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/99/4329984.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_4329984
loop_
_publ_author_name
'Romain J. Adcock'
'Duc Hanh Nguyen'
'Sonia Ladeira'
'Carole Le Berre'
'Philippe Serp'
'Philippe Kalck'
_publ_section_title
;
 Reactivity of Rhodium(I) Complexes Bearing Nitrogen-Containing Ligands
 toward CH3I: Synthesis and Full Characterization of Neutral
 cis-[RhX(CO)2(L)] and Acetyl [RhI(μ-I)(COMe)(CO)(L)]2 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8670
_journal_page_last               8685
_journal_paper_doi               10.1021/ic2019988
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C14 H18 I4 N4 O4 Rh2'
_chemical_formula_sum            'C14 H18 I4 N4 O4 Rh2'
_chemical_formula_weight         1019.74
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                105.633(6)
_cell_angle_beta                 93.540(7)
_cell_angle_gamma                112.887(5)
_cell_formula_units_Z            2
_cell_length_a                   10.1933(15)
_cell_length_b                   11.5069(17)
_cell_length_c                   12.3739(18)
_cell_measurement_reflns_used    9619
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      30.61
_cell_measurement_theta_min      3.01
_cell_measurement_wavelength     0.71073
_cell_volume                     1264.8(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       ω-φ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30995
_diffrn_reflns_theta_full        30.66
_diffrn_reflns_theta_max         30.66
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.212
_exptl_absorpt_correction_T_max  0.6364
_exptl_absorpt_correction_T_min  0.5227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.678
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.675
_refine_diff_density_min         -1.93
_refine_diff_density_rms         0.16
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         7757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0319P)²+6.5935P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                6927
_reflns_number_total             7757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2019988_si_002_10.cif
_cod_data_source_block           6d1
_cod_database_code               4329984
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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 0.59616(3) 0.65868(3) 0.44827(2) 0.02135(6) Uani 1 1 d .
I2 I 0.30131(3) 0.44890(3) 0.41964(2) 0.02842(6) Uani 1 1 d .
Rh2 Rh 0.02540(3) 0.83982(3) 0.02083(2) 0.02034(6) Uani 1 1 d .
I3 I 0.16927(3) 1.10175(3) 0.12441(2) 0.02561(6) Uani 1 1 d .
I1 I 0.49203(4) 0.77576(3) 0.33065(3) 0.03650(7) Uani 1 1 d .
I4 I -0.12830(3) 0.58098(3) -0.08003(3) 0.03157(7) Uani 1 1 d .
N1 N 0.6320(4) 0.5425(3) 0.3005(3) 0.0239(6) Uani 1 1 d .
C9 C 0.8138(6) 0.8257(6) 0.4835(4) 0.0410(13) Uani 1 1 d .
N2 N 0.5894(4) 0.4071(4) 0.1261(3) 0.0274(7) Uani 1 1 d .
C4 C 0.7222(5) 0.4261(5) 0.1770(4) 0.0327(9) Uani 1 1 d .
H4 H 0.7839 0.3885 0.1436 0.039 Uiso 1 1 calc R
C5 C 0.7483(5) 0.5101(5) 0.2856(4) 0.0305(8) Uani 1 1 d .
H5 H 0.8326 0.5411 0.3418 0.037 Uiso 1 1 calc R
C1 C 0.5492(5) 0.7474(5) 0.5779(4) 0.0356(10) Uani 1 1 d .
C2 C 0.5382(4) 0.4775(4) 0.2024(3) 0.0256(7) Uani 1 1 d .
H2 H 0.447 0.4803 0.1882 0.031 Uiso 1 1 calc R
O1 O 0.5153(5) 0.7954(5) 0.6559(3) 0.0580(12) Uani 1 1 d .
N3 N 0.1584(4) 0.8500(3) -0.1030(3) 0.0244(6) Uani 1 1 d .
N4 N 0.2182(4) 0.8406(4) -0.2715(3) 0.0336(8) Uani 1 1 d .
C8 C 0.1096(5) 0.7980(5) -0.2145(4) 0.0295(8) Uani 1 1 d .
H8 H 0.012 0.7389 -0.2496 0.035 Uiso 1 1 calc R
O4 O 0.2773(4) 0.8305(5) 0.1130(4) 0.0524(11) Uani 1 1 d .
C12 C 0.1605(5) 0.8049(4) 0.1257(4) 0.0303(8) Uani 1 1 d .
O3 O -0.1806(4) 0.8386(5) 0.1827(4) 0.0534(11) Uani 1 1 d .
C11 C -0.1021(5) 0.8368(5) 0.1223(4) 0.0323(9) Uani 1 1 d .
C13 C 0.0984(6) 0.7466(5) 0.2166(4) 0.0373(10) Uani 1 1 d .
H13A H 0.1708 0.7291 0.257 0.056 Uiso 1 1 calc R
H13B H 0.0118 0.6631 0.1808 0.056 Uiso 1 1 calc R
H13C H 0.0722 0.8097 0.2709 0.056 Uiso 1 1 calc R
C3 C 0.5160(6) 0.3258(5) 0.0087(4) 0.0381(11) Uani 1 1 d .
H3A H 0.4259 0.3352 -0.0077 0.057 Uiso 1 1 calc R
H3B H 0.4934 0.2323 -0.0009 0.057 Uiso 1 1 calc R
H3C H 0.5793 0.3555 -0.0441 0.057 Uiso 1 1 calc R
O2 O 0.8872(4) 0.7870(4) 0.4328(4) 0.0575(11) Uani 1 1 d .
C10 C 0.8235(7) 0.9405(6) 0.5606(5) 0.0556(16) Uani 1 1 d .
H10A H 0.8218 0.9304 0.6367 0.083 Uiso 1 1 calc R
H10B H 0.7413 0.9586 0.5382 0.083 Uiso 1 1 calc R
H10C H 0.9143 1.0146 0.5621 0.083 Uiso 1 1 calc R
C14 C 0.2028(7) 0.8015(8) -0.3958(5) 0.0535(15) Uani 1 1 d .
H14A H 0.2204 0.7216 -0.4234 0.08 Uiso 1 1 calc R
H14B H 0.2732 0.8741 -0.4173 0.08 Uiso 1 1 calc R
H14C H 0.1044 0.7826 -0.43 0.08 Uiso 1 1 calc R
C7 C 0.3413(5) 0.9235(5) -0.1923(4) 0.0335(9) Uani 1 1 d .
H7 H 0.4349 0.9686 -0.2071 0.04 Uiso 1 1 calc R
C6 C 0.3044(4) 0.9291(4) -0.0882(4) 0.0294(8) Uani 1 1 d .
H6 H 0.3687 0.9793 -0.0167 0.035 Uiso 1 1 calc R
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 0 '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 0.006 '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
C1 Rh1 N1 174.69(19) . .
C1 Rh1 C9 91.1(2) . .
N1 Rh1 C9 94.08(15) . .
C1 Rh1 I1 88.81(16) . .
N1 Rh1 I1 92.25(10) . .
C9 Rh1 I1 89.48(11) . .
C1 Rh1 I2 87.21(16) . 2_666
N1 Rh1 I2 91.76(10) . 2_666
C9 Rh1 I2 90.13(11) . 2_666
I1 Rh1 I2 175.991(15) . 2_666
C1 Rh1 I2 83.93(16) . .
N1 Rh1 I2 90.85(9) . .
C9 Rh1 I2 175.06(11) . .
I1 Rh1 I2 90.580(17) . .
I2 Rh1 I2 89.469(16) 2_666 .
Rh1 I2 Rh1 90.530(16) 2_666 .
C11 Rh2 C12 92.78(19) . .
C11 Rh2 N3 174.42(17) . .
C12 Rh2 N3 92.73(16) . .
C11 Rh2 I4 89.26(15) . .
C12 Rh2 I4 90.96(12) . .
N3 Rh2 I4 91.58(9) . .
C11 Rh2 I3 88.58(15) . .
C12 Rh2 I3 90.59(12) . .
N3 Rh2 I3 90.43(9) . .
I4 Rh2 I3 177.402(14) . .
C11 Rh2 I3 86.09(14) . 2_575
C12 Rh2 I3 178.06(12) . 2_575
N3 Rh2 I3 88.39(9) . 2_575
I4 Rh2 I3 90.600(16) . 2_575
I3 Rh2 I3 87.815(16) . 2_575
Rh2 I3 Rh2 92.185(15) . 2_575
C2 N1 C5 106.0(3) . .
C2 N1 Rh1 124.9(3) . .
C5 N1 Rh1 129.0(3) . .
O2 C9 C10 138.8(7) . .
O2 C9 Rh1 108.3(4) . .
C10 C9 Rh1 112.9(4) . .
C2 N2 C4 108.1(3) . .
C2 N2 C3 125.7(4) . .
C4 N2 C3 126.3(4) . .
C5 C4 N2 106.2(4) . .
C5 C4 H4 126.9 . .
N2 C4 H4 126.9 . .
C4 C5 N1 108.9(4) . .
C4 C5 H5 125.6 . .
N1 C5 H5 125.6 . .
O1 C1 Rh1 176.7(5) . .
N1 C2 N2 110.8(4) . .
N1 C2 H2 124.6 . .
N2 C2 H2 124.6 . .
C8 N3 C6 106.4(4) . .
C8 N3 Rh2 124.4(3) . .
C6 N3 Rh2 128.1(3) . .
C8 N4 C7 107.5(4) . .
C8 N4 C14 124.9(4) . .
C7 N4 C14 127.5(4) . .
N3 C8 N4 110.4(4) . .
N3 C8 H8 124.8 . .
N4 C8 H8 124.8 . .
O4 C12 C13 123.5(4) . .
O4 C12 Rh2 119.1(4) . .
C13 C12 Rh2 117.4(3) . .
O3 C11 Rh2 177.3(5) . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
N2 C3 H3A 109.5 . .
N2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
N2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N4 C14 H14A 109.5 . .
N4 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
N4 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C6 C7 N4 106.8(4) . .
C6 C7 H7 126.6 . .
N4 C7 H7 126.6 . .
C7 C6 N3 108.8(4) . .
C7 C6 H6 125.6 . .
N3 C6 H6 125.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 C1 1.854(4) .
Rh1 N1 2.100(3) .
Rh1 C9 2.217(6) .
Rh1 I1 2.6530(5) .
Rh1 I2 2.6800(5) 2_666
Rh1 I2 2.9581(6) .
I2 Rh1 2.6799(5) 2_666
Rh2 C11 1.859(5) .
Rh2 C12 2.057(5) .
Rh2 N3 2.105(3) .
Rh2 I4 2.6474(6) .
Rh2 I3 2.6694(6) .
Rh2 I3 2.9780(5) 2_575
I3 Rh2 2.9780(5) 2_575
N1 C2 1.326(5) .
N1 C5 1.383(5) .
C9 O2 1.149(6) .
C9 C10 1.368(8) .
N2 C2 1.340(5) .
N2 C4 1.367(6) .
N2 C3 1.461(5) .
C4 C5 1.367(6) .
C4 H4 0.95 .
C5 H5 0.95 .
C1 O1 1.121(6) .
C2 H2 0.95 .
N3 C8 1.322(5) .
N3 C6 1.378(5) .
N4 C8 1.351(6) .
N4 C7 1.363(6) .
N4 C14 1.461(6) .
C8 H8 0.95 .
O4 C12 1.142(6) .
C12 C13 1.509(6) .
O3 C11 1.130(6) .
C13 H13A 0.98 .
C13 H13B 0.98 .
C13 H13C 0.98 .
C3 H3A 0.98 .
C3 H3B 0.98 .
C3 H3C 0.98 .
C10 H10A 0.98 .
C10 H10B 0.98 .
C10 H10C 0.98 .
C14 H14A 0.98 .
C14 H14B 0.98 .
C14 H14C 0.98 .
C7 C6 1.356(6) .
C7 H7 0.95 .
C6 H6 0.95 .
