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
Romain J. Adcock; Duc Hanh Nguyen; Sonia Ladeira; Carole Le Berre; Philippe Serp; Philippe Kalck; Inorganic Chemistry 51 (2012) 8670–8685; doi:10.1021/ic2019988

data_4329983
_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(\m-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
;
 ?
;
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_atom_sites_solution_secondary   difmap
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_cell_angle_gamma                90
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_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       \w-\f
_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
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_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
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_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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0388P)^2^+3.6754P] where P=(Fo^2^+2Fc^2^)/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