#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:58:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179402 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/99/4329983.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_4329983
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_absolute_configuration ad
_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           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9689(2)
_cell_length_b                   20.4498(3)
_cell_length_c                   7.52620(10)
_cell_measurement_reflns_used    16049
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.2007
_cell_measurement_theta_min      3.3543
_cell_measurement_wavelength     0.71073
_cell_volume                     2457.76(6)
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction Ltd.'
_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    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       ω-φ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            23523
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.6
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.393
_exptl_absorpt_correction_T_max  0.528
_exptl_absorpt_correction_T_min  0.200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.756
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       0.00249(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4494
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0388P)²+3.6754P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.055
_refine_ls_wR_factor_ref         0.0551
_reflns_number_gt                4456
_reflns_number_total             4494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2019988_si_002_09.cif
_cod_data_source_block           6d2
_cod_database_code               4329983
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'
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
C1 C 0.4416(4) 0.3743(3) 0.3557(8) 0.0235(12) Uani 1 1 d .
C2 C 0.2153(3) 0.4081(3) -0.0698(8) 0.0211(11) Uani 1 1 d .
H2 H 0.2376 0.451 -0.0789 0.025 Uiso 1 1 calc R
C4 C 0.1387(4) 0.3215(3) -0.1183(8) 0.0258(12) Uani 1 1 d .
H4 H 0.0981 0.2925 -0.1661 0.031 Uiso 1 1 calc R
C5 C 0.1944(3) 0.3085(3) 0.0104(8) 0.0237(11) Uani 1 1 d .
H5 H 0.1996 0.268 0.071 0.028 Uiso 1 1 calc R
C3 C 0.1062(4) 0.4225(3) -0.3031(9) 0.0342(14) Uani 1 1 d .
H3A H 0.1209 0.4689 -0.2947 0.051 Uiso 1 1 calc R
H3B H 0.0459 0.4172 -0.2842 0.051 Uiso 1 1 calc R
H3C H 0.1212 0.406 -0.4211 0.051 Uiso 1 1 calc R
C9 C 0.2878(3) 0.4443(3) 0.3519(8) 0.0236(12) Uani 1 1 d .
C10 C 0.3278(4) 0.4682(3) 0.5203(10) 0.0339(13) Uani 1 1 d .
H10A H 0.2913 0.5007 0.5767 0.051 Uiso 1 1 calc R
H10B H 0.382 0.4882 0.4927 0.051 Uiso 1 1 calc R
H10C H 0.3362 0.4313 0.6014 0.051 Uiso 1 1 calc R
C11 C 0.4777(4) 0.2016(3) 0.3888(8) 0.0259(12) Uani 1 1 d .
C8 C 0.2587(4) 0.1468(3) -0.0415(7) 0.0229(12) Uani 1 1 d .
H8 H 0.301 0.1505 -0.1298 0.027 Uiso 1 1 calc R
C7 C 0.1363(4) 0.1355(3) 0.0849(8) 0.0247(13) Uani 1 1 d .
H7 H 0.078 0.13 0.1043 0.03 Uiso 1 1 calc R
C6 C 0.1960(3) 0.1411(2) 0.2102(8) 0.0225(11) Uani 1 1 d .
H6 H 0.1864 0.1402 0.3347 0.027 Uiso 1 1 calc R
C14 C 0.1370(4) 0.1370(4) -0.2496(9) 0.0378(16) Uani 1 1 d .
H14A H 0.0783 0.1505 -0.2395 0.057 Uiso 1 1 calc R
H14B H 0.1397 0.0922 -0.2959 0.057 Uiso 1 1 calc R
H14C H 0.1665 0.1665 -0.3309 0.057 Uiso 1 1 calc R
C12 C 0.4521(4) 0.1041(3) 0.1261(8) 0.0226(11) Uani 1 1 d .
C13 C 0.5337(4) 0.0809(3) 0.2059(9) 0.0292(13) Uani 1 1 d .
H13A H 0.5565 0.0452 0.1335 0.044 Uiso 1 1 calc R
H13B H 0.5238 0.0652 0.3271 0.044 Uiso 1 1 calc R
H13C H 0.5738 0.1171 0.2087 0.044 Uiso 1 1 calc R
N1 N 0.2429(3) 0.36283(19) 0.0413(6) 0.0189(9) Uani 1 1 d .
N2 N 0.1523(3) 0.3855(2) -0.1666(6) 0.0224(10) Uani 1 1 d .
N3 N 0.2729(3) 0.1483(2) 0.1313(6) 0.0193(9) Uani 1 1 d .
N4 N 0.1762(3) 0.1394(2) -0.0762(7) 0.0227(10) Uani 1 1 d .
O1 O 0.5007(3) 0.3734(2) 0.4360(7) 0.0353(10) Uani 1 1 d .
O2 O 0.2231(3) 0.4660(2) 0.2983(7) 0.0462(13) Uani 1 1 d .
O3 O 0.5319(3) 0.2201(2) 0.4722(7) 0.0422(12) Uani 1 1 d .
O4 O 0.4249(3) 0.0840(2) -0.0081(7) 0.0401(12) Uani 1 1 d .
Rh1 Rh 0.34597(2) 0.371532(18) 0.21435(6) 0.01556(9) Uani 1 1 d .
Rh2 Rh 0.38520(2) 0.173863(18) 0.25906(6) 0.01577(10) Uani 1 1 d .
I1 I 0.41952(2) 0.461253(16) 0.01101(6) 0.02534(9) Uani 1 1 d .
I2 I 0.28686(2) 0.283019(16) 0.44502(5) 0.02243(9) Uani 1 1 d .
I3 I 0.422171(19) 0.263065(15) 0.01034(5) 0.02031(9) Uani 1 1 d .
I4 I 0.35477(2) 0.088382(16) 0.51381(5) 0.02466(10) Uani 1 1 d .
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
O1 C1 Rh1 176.5(5)
N1 C2 N2 110.9(5)
N1 C2 H2 124.5
N2 C2 H2 124.5
C5 C4 N2 105.9(5)
C5 C4 H4 127
N2 C4 H4 127
C4 C5 N1 109.6(5)
C4 C5 H5 125.2
N1 C5 H5 125.2
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
O2 C9 C10 122.2(5)
O2 C9 Rh1 119.6(5)
C10 C9 Rh1 118.2(4)
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
O3 C11 Rh2 177.1(5)
N3 C8 N4 111.1(5)
N3 C8 H8 124.4
N4 C8 H8 124.4
C6 C7 N4 106.6(5)
C6 C7 H7 126.7
N4 C7 H7 126.7
C7 C6 N3 109.9(5)
C7 C6 H6 125.1
N3 C6 H6 125.1
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
O4 C12 C13 123.4(5)
O4 C12 Rh2 118.2(4)
C13 C12 Rh2 118.4(4)
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
C2 N1 C5 105.7(5)
C2 N1 Rh1 126.3(3)
C5 N1 Rh1 127.8(4)
C2 N2 C4 107.8(5)
C2 N2 C3 125.7(5)
C4 N2 C3 126.5(5)
C8 N3 C6 105.7(5)
C8 N3 Rh2 127.1(4)
C6 N3 Rh2 126.3(4)
C8 N4 C7 106.7(5)
C8 N4 C14 126.8(5)
C7 N4 C14 126.4(5)
C1 Rh1 C9 93.5(2)
C1 Rh1 N1 175.3(2)
C9 Rh1 N1 91.1(2)
C1 Rh1 I1 86.89(18)
C9 Rh1 I1 89.43(16)
N1 Rh1 I1 92.71(12)
C1 Rh1 I2 86.52(18)
C9 Rh1 I2 90.20(16)
N1 Rh1 I2 93.93(12)
I1 Rh1 I2 173.36(2)
C1 Rh1 I3 88.95(18)
C9 Rh1 I3 177.15(16)
N1 Rh1 I3 86.39(12)
I1 Rh1 I3 92.113(16)
I2 Rh1 I3 88.549(14)
C11 Rh2 C12 93.1(2)
C11 Rh2 N3 173.9(2)
C12 Rh2 N3 92.8(2)
C11 Rh2 I4 88.11(18)
C12 Rh2 I4 89.43(16)
N3 Rh2 I4 90.61(13)
C11 Rh2 I3 89.08(18)
C12 Rh2 I3 91.01(16)
N3 Rh2 I3 92.16(13)
I4 Rh2 I3 177.18(2)
C11 Rh2 I2 86.83(17)
C12 Rh2 I2 177.34(16)
N3 Rh2 I2 87.30(12)
I4 Rh2 I2 93.226(15)
I3 Rh2 I2 86.338(13)
Rh1 I2 Rh2 90.897(14)
Rh2 I3 Rh1 93.279(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 O1 1.120(7)
C1 Rh1 1.863(6)
C2 N1 1.323(7)
C2 N2 1.325(7)
C2 H2 0.95
C4 C5 1.342(8)
C4 N2 1.376(7)
C4 H4 0.95
C5 N1 1.373(7)
C5 H5 0.95
C3 N2 1.472(7)
C3 H3A 0.98
C3 H3B 0.98
C3 H3C 0.98
C9 O2 1.194(7)
C9 C10 1.501(9)
C9 Rh1 2.037(6)
C10 H10A 0.98
C10 H10B 0.98
C10 H10C 0.98
C11 O3 1.133(7)
C11 Rh2 1.860(6)
C8 N3 1.321(8)
C8 N4 1.352(7)
C8 H8 0.95
C7 C6 1.346(9)
C7 N4 1.372(8)
C7 H7 0.95
C6 N3 1.371(7)
C6 H6 0.95
C14 N4 1.449(8)
C14 H14A 0.98
C14 H14B 0.98
C14 H14C 0.98
C12 O4 1.174(7)
C12 C13 1.512(8)
C12 Rh2 2.044(5)
C13 H13A 0.98
C13 H13B 0.98
C13 H13C 0.98
N1 Rh1 2.106(4)
N3 Rh2 2.101(5)
Rh1 I1 2.6624(5)
Rh1 I2 2.6797(5)
Rh1 I3 2.9595(5)
Rh2 I4 2.6397(5)
Rh2 I3 2.6796(5)
Rh2 I2 3.0672(5)
