#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:58:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179402 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/99/4329982.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_4329982
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         'C6 H6 I N2 O2 Rh'
_chemical_formula_sum            'C6 H6 I N2 O2 Rh'
_chemical_formula_weight         367.94
_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                86.941(4)
_cell_angle_beta                 85.400(4)
_cell_angle_gamma                64.642(5)
_cell_formula_units_Z            4
_cell_length_a                   8.1648(4)
_cell_length_b                   9.3741(4)
_cell_length_c                   14.6087(7)
_cell_measurement_reflns_used    5201
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.5961
_cell_measurement_theta_min      3.6448
_cell_measurement_wavelength     0.71073
_cell_volume                     1006.91(9)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0356
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15125
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.726
_exptl_absorpt_correction_T_max  0.695
_exptl_absorpt_correction_T_min  0.510
_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            yellow
_exptl_crystal_density_diffrn    2.427
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.1
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0218P)²+0.1913P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.049
_refine_ls_wR_factor_ref         0.0521
_reflns_number_gt                3143
_reflns_number_total             3675
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2019988_si_002_08.cif
_cod_data_source_block           4f
_cod_database_code               4329982
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
C1 C 0.2414(6) 0.5312(5) 0.6132(3) 0.0370(10) Uani 1 1 d .
C2 C -0.0283(6) 0.6033(5) 0.7382(3) 0.0356(10) Uani 1 1 d .
C3 C -0.5570(6) 0.9764(5) 0.6106(3) 0.0394(11) Uani 1 1 d .
H3 H -0.6484 1.0816 0.6146 0.047 Uiso 1 1 calc R
C4 C -0.5848(6) 0.8475(5) 0.5936(3) 0.0396(10) Uani 1 1 d .
H4 H -0.6967 0.8438 0.584 0.047 Uiso 1 1 calc R
C5 C -0.4134(6) 0.7225(5) 0.5936(3) 0.0350(10) Uani 1 1 d .
H5 H -0.3884 0.6156 0.5835 0.042 Uiso 1 1 calc R
C6 C -0.2875(7) 1.0256(5) 0.6404(3) 0.0478(12) Uani 1 1 d .
H6A H -0.3686 1.1377 0.6319 0.072 Uiso 1 1 calc R
H6B H -0.1788 0.998 0.5987 0.072 Uiso 1 1 calc R
H6C H -0.2522 1.0053 0.704 0.072 Uiso 1 1 calc R
C7 C 1.1129(6) -0.0817(5) 0.8220(3) 0.0367(10) Uani 1 1 d .
C8 C 1.1515(6) 0.1825(5) 0.8195(3) 0.0395(10) Uani 1 1 d .
C9 C 0.6118(6) 0.5887(5) 0.9360(3) 0.0381(10) Uani 1 1 d .
H9 H 0.5104 0.6858 0.9246 0.046 Uiso 1 1 calc R
C10 C 0.7208(6) 0.5550(5) 1.0077(3) 0.0418(11) Uani 1 1 d .
H10 H 0.7102 0.6232 1.0558 0.05 Uiso 1 1 calc R
C11 C 0.8498(6) 0.4011(5) 0.9959(3) 0.0357(10) Uani 1 1 d .
H11 H 0.9453 0.3458 1.0353 0.043 Uiso 1 1 calc R
C12 C 0.6047(6) 0.4374(5) 0.8010(3) 0.0434(11) Uani 1 1 d .
H12A H 0.508 0.5378 0.7816 0.065 Uiso 1 1 calc R
H12B H 0.5559 0.3585 0.812 0.065 Uiso 1 1 calc R
H12C H 0.7031 0.401 0.7527 0.065 Uiso 1 1 calc R
O1 O 0.3938(4) 0.4590(4) 0.6147(2) 0.0536(9) Uani 1 1 d .
O2 O -0.0341(5) 0.5763(4) 0.8140(2) 0.0533(9) Uani 1 1 d .
O7 O 1.1989(5) -0.2052(4) 0.7962(2) 0.0537(9) Uani 1 1 d .
O8 O 1.2609(5) 0.2201(4) 0.7902(2) 0.0530(8) Uani 1 1 d .
Rh2 Rh 0.97597(4) 0.11829(4) 0.86573(2) 0.03151(9) Uani 1 1 d .
Rh1 Rh -0.00646(4) 0.64447(4) 0.61331(2) 0.02963(9) Uani 1 1 d .
I1 I 0.04009(4) 0.72059(3) 0.438259(18) 0.03543(8) Uani 1 1 d .
I2 I 0.72525(4) 0.01977(3) 0.925820(19) 0.04162(9) Uani 1 1 d .
N1 N -0.2889(4) 0.7729(4) 0.6098(2) 0.0289(7) Uani 1 1 d .
N2 N -0.3802(5) 0.9311(4) 0.6206(2) 0.0317(8) Uani 1 1 d .
N3 N 0.8204(5) 0.3421(4) 0.9211(2) 0.0323(8) Uani 1 1 d .
N4 N 0.6742(5) 0.4592(4) 0.8847(2) 0.0332(8) 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'
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'
N N 0.0061 0.0033 '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 178.4(4)
O2 C2 Rh1 177.2(4)
N2 C3 C4 109.0(4)
N2 C3 H3 125.5
C4 C3 H3 125.5
C3 C4 C5 104.6(4)
C3 C4 H4 127.7
C5 C4 H4 127.7
N1 C5 C4 110.7(4)
N1 C5 H5 124.6
C4 C5 H5 124.6
N2 C6 H6A 109.5
N2 C6 H6B 109.5
H6A C6 H6B 109.5
N2 C6 H6C 109.5
H6A C6 H6C 109.5
H6B C6 H6C 109.5
O7 C7 Rh2 178.9(4)
O8 C8 Rh2 179.0(4)
N4 C9 C10 107.3(4)
N4 C9 H9 126.3
C10 C9 H9 126.3
C9 C10 C11 106.0(4)
C9 C10 H10 127
C11 C10 H10 127
N3 C11 C10 110.0(4)
N3 C11 H11 125
C10 C11 H11 125
N4 C12 H12A 109.5
N4 C12 H12B 109.5
H12A C12 H12B 109.5
N4 C12 H12C 109.5
H12A C12 H12C 109.5
H12B C12 H12C 109.5
C7 Rh2 C8 90.73(18)
C7 Rh2 N3 177.59(15)
C8 Rh2 N3 90.48(15)
C7 Rh2 I2 87.54(13)
C8 Rh2 I2 177.64(12)
N3 Rh2 I2 91.31(9)
C1 Rh1 C2 90.22(18)
C1 Rh1 N1 178.54(15)
C2 Rh1 N1 91.14(16)
C1 Rh1 I1 87.78(13)
C2 Rh1 I1 174.55(12)
N1 Rh1 I1 90.91(8)
C5 N1 N2 105.9(3)
C5 N1 Rh1 129.1(3)
N2 N1 Rh1 124.9(2)
C3 N2 N1 109.7(3)
C3 N2 C6 129.0(4)
N1 N2 C6 121.3(3)
C11 N3 N4 106.0(3)
C11 N3 Rh2 127.6(3)
N4 N3 Rh2 126.4(2)
C9 N4 N3 110.7(3)
C9 N4 C12 128.1(4)
N3 N4 C12 121.2(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 O1 1.135(5)
C1 Rh1 1.839(5)
C2 O2 1.125(5)
C2 Rh1 1.855(4)
C3 N2 1.337(5)
C3 C4 1.360(6)
C3 H3 0.95
C4 C5 1.388(6)
C4 H4 0.95
C5 N1 1.332(5)
C5 H5 0.95
C6 N2 1.441(5)
C6 H6A 0.98
C6 H6B 0.98
C6 H6C 0.98
C7 O7 1.133(5)
C7 Rh2 1.841(4)
C8 O8 1.140(5)
C8 Rh2 1.847(5)
C9 N4 1.342(5)
C9 C10 1.364(6)
C9 H9 0.95
C10 C11 1.384(6)
C10 H10 0.95
C11 N3 1.333(5)
C11 H11 0.95
C12 N4 1.448(5)
C12 H12A 0.98
C12 H12B 0.98
C12 H12C 0.98
Rh2 N3 2.099(3)
Rh2 I2 2.6568(4)
Rh1 N1 2.099(3)
Rh1 I1 2.6599(4)
N1 N2 1.357(4)
N3 N4 1.353(4)
